CN108690596B - Crosslinking accelerator for hydrocarbon anhydrous fracturing fluid and hydrocarbon anhydrous fracturing fluid - Google Patents
Crosslinking accelerator for hydrocarbon anhydrous fracturing fluid and hydrocarbon anhydrous fracturing fluid Download PDFInfo
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Abstract
The invention discloses a crosslinking accelerator for a carbon hydrocarbon anhydrous fracturing fluid, wherein each 100mL of the crosslinking accelerator contains 3g to 10g of alkali metal hydroxide, 0.6g to 1.5g of ferric sulfate and 50mL to 90mL of organic alcohol; the organic alcohol is one or more of ethanol, ethylene glycol and propylene glycol. In addition, the invention also provides a hydrocarbon anhydrous fracturing fluid prepared by the crosslinking accelerator, which comprises a base fluid, a gelling agent and the crosslinking accelerator; the carbon hydrocarbon anhydrous fracturing fluid is gelled, is broken, is added with a gelling accelerator and a gelling agent, and can form a secondary utilization fracturing fluid. The crosslinking accelerator can effectively improve the viscosity and gelling property of the fracturing fluid, improve the temperature resistance, the shearing resistance and the gel breaking capacity of the fracturing fluid, can be reused after gel breaking, has good temperature resistance, and is beneficial to development and application in unconventional reservoirs.
Description
Technical Field
The invention belongs to the technical field of oilfield chemistry and fracturing yield increase, and particularly relates to a crosslinking accelerator for a carbon hydrocarbon anhydrous fracturing fluid and the carbon hydrocarbon anhydrous fracturing fluid.
Background
At present, the demand of oil gas is increasing day by day, and the output of conventional oil gas is decreasing continuously, so unconventional oil gas resources such as compact sandstone gas, coal bed gas and shale gas have attracted high attention from countries all over the world. The unconventional oil and gas resources in China are very rich, but unconventional oil and gas reservoirs have the characteristics of low porosity, low permeability and poor physical properties of the reservoirs and usually show very strong water sensitivity, and the conventional water-based fracturing fluid is very easy to cause water lock on the reservoirs, so that the permeability of the reservoirs is reduced, the reservoirs are damaged, and the fracturing effect is influenced. The anhydrous fracturing basically does not need water in the whole fracturing process, wherein the oil-based fracturing fluid is an ideal fracturing fluid system suitable for water-sensitive, acid-sensitive, low-permeability and low-energy strata, and has development values in process, technology and economy.
The domestic oil-based fracturing fluid mainly comprises crude oil, a gelling agent, a gel breaker and the like, wherein the gelling agent is a key component in the fracturing fluid, and because certain corresponding relation exists between alkyl carbon chain distribution in the structure of the gelling agent and the selected crude oil or diesel oil, the quality of the fracturing fluid is directly influenced by the performance of the gelling agent.
At present, oil-based fracturing fluid systems at home and abroad are developing towards the directions of strong adaptability, low cost, high temperature resistance and environmental protection, and a continuously constructed fracturing fluid system suitable for low-permeability, high-temperature or strong water-sensitive strata is formed. But the research and application of the low-damage continuous construction fracturing fluid system in China are still in the starting stage. The controllability of the gelling time and the expansion of the temperature resistance range of the fracturing fluid are important measures for promoting the fracturing fluid system to be suitable for different operation conditions. Meanwhile, the gelling process of the fracturing fluid is simplified, so that the construction process is simplified, and the key measure for reducing the fracturing construction cost is provided.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a crosslinking accelerator for a hydrocarbon anhydrous fracturing fluid and a hydrocarbon anhydrous fracturing fluid prepared by using the crosslinking accelerator, aiming at the defects of the prior art. The crosslinking accelerator can effectively improve the viscosity and gelling property of the fracturing fluid, improve the temperature resistance, the shearing resistance and the gel breaking capacity of the fracturing fluid, can be reused after gel breaking, has good temperature resistance, and is beneficial to development and application in unconventional reservoirs.
In order to solve the technical problems, the invention adopts the technical scheme that: a crosslinking accelerator for a carbon hydrocarbon anhydrous fracturing fluid is characterized in that every 100mL of the crosslinking accelerator contains 3g to 10g of alkali metal hydroxide, 0.6g to 1.5g of ferric sulfate and 50mL to 90mL of organic alcohol; the organic alcohol is one or more of ethanol, ethylene glycol and propylene glycol; the alkali metal hydroxide is sodium hydroxide or potassium hydroxide.
The crosslinking accelerator for the carbon hydrocarbon anhydrous fracturing fluid is characterized in that the organic alcohol is a mixture of ethylene glycol and ethanol, and the volume ratio of the ethylene glycol to the ethanol is 1 (0.5-2).
The crosslinking accelerator for the carbon-hydrocarbon anhydrous fracturing fluid is characterized in that each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 1g of ferric sulfate, 20mL of ethanol, 40mL of glycol and the balance of water.
The invention also provides a hydrocarbon anhydrous fracturing fluid prepared by adopting the crosslinking accelerator, which is characterized by comprising base fluid, a gelling agent and the crosslinking accelerator, wherein the volume of the gelling agent is 3-5% of that of the base fluid, the volume of the crosslinking accelerator is 1-3% of that of the base fluid, the gelling agent is a gelling agent phosphate aluminum oil-based fracturing fluid gelling agent disclosed in the invention patent with the patent number of ZL00100278.3 and the name of 'a phosphate aluminum oil-based fracturing fluid gelling agent and a preparation method thereof'; the base liquid is diesel oil, crude oil, kerosene, hexane, pentane or propane;
the hydrocarbon anhydrous fracturing fluid is characterized in that the volume of the gelling agent in the hydrocarbon anhydrous fracturing fluid is 4% of the volume of the base fluid, and the volume of the crosslinking accelerator is 2.4% of the volume of the base fluid.
The carbon hydrocarbon anhydrous fracturing fluid is characterized in that the carbon hydrocarbon anhydrous fracturing fluid is gelled and then is broken by a gel breaker to form a gel breaking liquid, and the gel breaking liquid is mixed with the gelling agent and a gelling accelerator to be used as a fracturing fluid for secondary utilization; the volume of the gelatinizing agent is 0.5-2% of the volume of the gel breaking liquid, the volume of the re-gelatinizing accelerant is 7-11% of the volume of the gel breaking liquid, and the re-gelatinizing accelerant is a mixed solution of absolute ethyl alcohol and concentrated sulfuric acid with the mass concentration of 98.3% according to the volume ratio of 9 (0.5-1.5).
The carbon hydrocarbon anhydrous fracturing fluid is characterized in that the gel breaker is sodium acetate, and the dosage of the gel breaker is 0.8-2.4 g per 100mL of the carbon hydrocarbon anhydrous fracturing fluid.
Compared with the prior art, the invention has the following advantages:
1. the crosslinking accelerator for the carbon hydrocarbon anhydrous fracturing fluid can effectively improve the viscosity and the gelling performance of the fracturing fluid, ferric sulfate in the crosslinking accelerator can increase the viscosity of the fracturing fluid, and the gelling time of the fracturing fluid can be controlled by adjusting the proportion of organic alcohol in the crosslinking accelerator. The fracturing fluid prepared by the crosslinking accelerant of the invention has improved temperature resistance, shear resistance and gel breaking capability, and can meet different requirements of different site operations on the fracturing fluid.
2. When the volume of the gelling agent is 4 percent of that of the diesel oil, the volume of the crosslinking accelerator is 2.4 percent of that of the diesel oil, and each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 1g of ferric sulfate, 20mL of ethanol and 40mL of ethylene glycol, the fracturing fluid has the optimal temperature resistance and shear resistance. The fracturing fluid can form jelly in 1min, and is prepared at 120 deg.C for 170s-1After 120min of continuous shearing, the viscosity of the fracturing fluid is 125mPa.s, and the fracturing fluid also has high recoverability, under the condition of unchanged temperature, the viscosity is gradually reduced along with the increase of the shear rate, and when the shear rate is reduced, the viscosity is slowly recovered to the level before shearing.
3. The carbon hydrocarbon anhydrous fracturing fluid prepared by the crosslinking accelerant can be repeatedly utilized after gel breaking. The gelling agent and the gelling accelerator are added into the gel breaking liquid of the fracturing fluid to obtain the secondary utilization fracturing fluid, and the obtained secondary utilization fracturing fluid basically recovers the temperature resistance before gel breaking.
4. The fracturing fluid can effectively reduce the economic cost of the oil-based fracturing fluid and expand the development and application of the oil-based fracturing fluid in unconventional reservoirs.
The technical solution of the present invention is further described in detail with reference to the accompanying drawings and embodiments.
Drawings
FIG. 1 is a graph showing the evaluation of the shear resistance of a hydrocarbon anhydrous fracturing fluid of example 5 of the present invention.
FIG. 2 is a graph showing the evaluation of the thermal resistance of the hydrocarbon-based anhydrous fracturing fluid of example 5 of the present invention.
Fig. 3 is a graph showing the evaluation of the temperature resistance of the hydrocarbon anhydrous fracturing fluid of example 12 of the present invention.
Fig. 4 is a graph showing the evaluation of the shear resistance of the hydrocarbon anhydrous fracturing fluid of example 12 of the present invention.
Fig. 5 is a graph showing the evaluation of the temperature resistance of the secondary fracturing fluid in example 20 of the present invention.
Detailed Description
Example 1
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 10g of sodium hydroxide, 3g of a 20% ferric sulfate solution, 45mL of ethanol, 45mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 4% of that of the diesel oil, and the volume of the crosslinking accelerator is 2% of that of the diesel oil, wherein the gelling agent is an oil-based fracturing fluid gelling agent which is prepared by adding toluene into dialkyl aluminum phosphate in example 1 and has the mass content of 50% and is disclosed in the invention patent with the patent number of ZL00100278.3 and the name of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof'.
Example 2
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 10g of sodium hydroxide, 5g of a 20% ferric sulfate solution, 45mL of ethanol, 45mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 4% of that of the diesel oil, and the volume of the crosslinking accelerator is 2% of that of the diesel oil, wherein the gelling agent is an oil-based fracturing fluid gelling agent which is prepared by adding toluene into dialkyl aluminum phosphate in example 1 and has the mass content of 80% and is disclosed in the invention patent with the patent number of ZL00100278.3 and the name of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof'.
Example 3
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 10g of sodium hydroxide, 7.5g of a 20% ferric sulfate solution, 45mL of ethanol, 45mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 4% of that of the diesel oil, and the volume of the crosslinking accelerator is 2% of that of the diesel oil, wherein the gelling agent is an oil-based fracturing fluid gelling agent which is prepared by adding toluene into dialkyl aluminum phosphate in example 1 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof' and has the patent number of ZL 00100278.3.
Comparative example 1
According to the crosslinking accelerator for the anhydrous fracturing of the hydrocarbon, each 100mL of the crosslinking accelerator contains 10g of sodium hydroxide, 45mL of ethanol, 45mL of glycol and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The carbon hydrocarbon anhydrous fracturing fluid prepared by using the crosslinking accelerator of the comparative example comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 4% of that of the diesel oil, and the volume of the crosslinking accelerator is 2% of that of the diesel oil, wherein the gelling agent is an oil-based fracturing fluid gelling agent which is prepared by adding toluene into dialkyl aluminum phosphate in example 1 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof' and has the patent number of ZL 00100278.3.
The gel forming time, viscosity and temperature resistance of the hydrocarbon anhydrous fracturing fluids of example 1, example 2, example 3 and comparative example 1 were measured. The gelling time is determined by a stopwatch, the fracturing fluid is placed in a magnetic stirrer, the stopwatch is pressed while the magnetic stirrer is started, and the time required for vortex disappearance and the time required for the fracturing fluid to become gel are respectively recorded; the viscosity of the fracturing fluid was measured by a Hakke rotational viscometer. The results are shown in tables 1 and 2.
TABLE 1 Effect of different iron sulfate additions on gel formation time and viscosity
TABLE 2 influence of iron sulfate addition on temperature resistance of fracturing fluids
As shown in tables 1 and 2, the addition of ferric sulfate can greatly increase the viscosity of the fracturing fluid, and the fracturing fluid of example 2 has higher viscosity and better temperature resistance.
Example 4
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 5g of a 20% ferric sulfate solution, 20mL of ethanol, 40mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by using the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 4% of that of the diesel oil, and the volume of the crosslinking accelerator is 1.0% of that of the diesel oil, wherein the gelling agent is an oil-based fracturing fluid gelling agent which is prepared by adding toluene into dialkyl aluminum phosphate in example 2 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof' and has the patent number of ZL 00100278.3.
Example 5
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 5g of ferric sulfate with a mass content of 20%, 20mL of ethanol, 40mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 4% of that of the diesel oil, and the volume of the crosslinking accelerator is 2.4% of that of the diesel oil, wherein the gelling agent is an oil-based fracturing fluid gelling agent with the mass content of 80% of dialkyl aluminum phosphate prepared by adding toluene into dialkyl aluminum phosphate in example 2 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof'.
As can be seen from FIG. 1, the shear rate was 170s at a test temperature of 120 ℃ C-1When the fracturing fluid is subjected to continuous shearing for 120min, the viscosity of the fracturing fluid corresponding to the embodiment 5 is 125mPa & s; as can be seen in FIG. 2, at 170s-1At a shear rate of 40 ℃ to 120 ℃, examples5 has a viscosity of about 200 mPas.
Example 6
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 5g of a 20% ferric sulfate solution, 20mL of ethanol, 40mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 4% of that of the diesel oil, and the volume of the crosslinking accelerator is 3.0% of that of the diesel oil, wherein the gelling agent is an oil-based fracturing fluid gelling agent with the mass content of 50% of dialkyl aluminum phosphate prepared by adding toluene into dialkyl aluminum phosphate in example 2 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof'.
The gelling time, viscosity and temperature resistance of the hydrocarbon-based anhydrous fracturing fluids of example 4, example 5 and example 6 were measured. The gelling time is determined by a stopwatch, the fracturing fluid is placed in a magnetic stirrer, the stopwatch is pressed while the magnetic stirrer is started, and the time required for vortex disappearance and the time required for the fracturing fluid to become gel are respectively recorded; the viscosity of the fracturing fluid was measured by a Hakke rotational viscometer. The results are shown in Table 3.
TABLE 3 Effect of volume of different crosslinking promoters in Diesel oil on gel time and viscosity
As can be seen from table 3, the change in the amount of the crosslinking accelerator added can cause the viscosity of the fracturing fluid to change, and as the amount of the crosslinking accelerator added increases, the viscosity of the fracturing fluid tends to increase first and then decrease, and the gel formation time decreases as the amount of the crosslinking accelerator added increases.
Example 7
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 5g of potassium hydroxide, 5g of a 20% ferric sulfate solution, 20mL of ethylene glycol, 40mL of ethanol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon and hydrocarbon prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is crude oil, the volume of the gelling agent is 3% of that of the crude oil, and the volume of the crosslinking accelerator is 2.4% of that of the crude oil; the gelatinizer is an oil-based fracturing fluid gelatinizer which is prepared by adding methylbenzene into dialkyl aluminum phosphate in example 4 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelatinizer and a preparation method thereof' with the patent number of ZL 00100278.3.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 6.53s, and the fracturing fluid becomes jelly within 23.22 s; the viscosity was found to be 502.6 mPas.
Example 8
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 3g of sodium hydroxide, 5g of a 20% ferric sulfate solution, 50mL of propylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The hydrocarbon anhydrous fracturing fluid prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 5% of that of the diesel oil, and the volume of the crosslinking accelerator is 2.4% of that of the diesel oil; the gelling agent is an oil-based fracturing fluid gelling agent which is prepared by adding toluene into dialkyl aluminum phosphate in example 4 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof' with the patent number of ZL00100278.3, wherein the mass content of the dialkyl aluminum phosphate is 40%.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 9.12s, and the fracturing fluid becomes jelly within 24.56 s; the viscosity was found to be 516.8 mPas.
Example 9
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 10g of sodium hydroxide, 5g of a 20% ferric sulfate solution, 50mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The hydrocarbon anhydrous fracturing fluid prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 5% of that of the diesel oil, and the volume of the crosslinking accelerator is 2.4% of that of the diesel oil; the gelling agent is an oil-based fracturing fluid gelling agent which is prepared by adding toluene into dialkyl aluminum phosphate in example 5 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof' with the patent number of ZL00100278.3, wherein the mass content of the dialkyl aluminum phosphate is 40%.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 10.72s, and the fracturing fluid becomes jelly within 31.14 s; the viscosity was found to be 618.8 mPas.
Example 10
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 3g of potassium hydroxide, 5g of a 20% ferric sulfate solution, 30mL of ethanol, 30mL of ethylene glycol and 30mL of propylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The hydrocarbon anhydrous fracturing fluid prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is diesel oil, the volume of the gelling agent is 5% of that of the diesel oil, and the volume of the crosslinking accelerator is 2.4% of that of the diesel oil; the gelatinizer is an oil-based fracturing fluid gelatinizer which is prepared by adding methylbenzene into dialkyl aluminum phosphate in example 5 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelatinizer and a preparation method thereof' with the patent number of ZL 00100278.3.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 5.44s, and the fracturing fluid becomes jelly within 22.32 s; the viscosity was found to be 632.6 mPas.
Example 11
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 5g of a 20% ferric sulfate solution, 50mL of ethanol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid of hydrocarbon prepared by the crosslinking accelerator comprises base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is kerosene, the volume of the gelling agent is 4% of that of the kerosene, and the volume of the crosslinking accelerator is 2.4% of that of the kerosene; the gelatinizer is an oil-based fracturing fluid gelatinizer which is prepared by adding toluene into dialkyl aluminum phosphate in example 5 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelatinizer and a preparation method thereof' with the patent number of ZL00100278.3, wherein the dialkyl aluminum phosphate is the oil-based fracturing fluid gelatinizer with the mass content of 50%.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 5.42s, and the fracturing fluid becomes jelly within 22.29 s; the viscosity was found to be 622.7 mPas.
Example 12
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 5g of potassium hydroxide, 5g of ferric sulfate with a mass content of 20%, 20mL of ethanol, 40mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by using the crosslinking accelerator comprises a base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is pentane, the volume of the gelling agent is 3% of that of the pentane, and the volume of the crosslinking accelerator is 2.4% of that of the pentane, wherein the gelling agent is an oil-based fracturing fluid gelling agent with the mass content of 80% of dialkyl aluminum phosphate prepared by adding toluene into dialkyl aluminum phosphate in example 4 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof'.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 5.04s, and the fracturing fluid becomes jelly within 22.41 s; the viscosity was found to be 632.7 mPas.
As can be seen from FIG. 3, the fracturing fluid of the present embodiment maintains a shear rate of 170S-1The temperature is continuously increased under the unchanged condition, the recording is carried out when the temperature reaches 95 ℃, the temperature is increased to 130 ℃ after 70min, and the viscosity of the fracturing fluid is reduced from 600 mPas (95 ℃) to 90 mPas (130 ℃). It can be seen from this that: the temperature resistance of the fracturing fluid system can reach 130 ℃. From FIG. 4, the fracturing fluid of this example was prepared at 110 ℃ for 170s-1After continuous shearing for 60min, the viscosity of the fracturing fluid is still more than 300 mPas.
Example 13
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 5g of ferric sulfate with a mass content of 20%, 20mL of ethanol, 40mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbon prepared by the crosslinking accelerator comprises a base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is pentane, the volume of the gelling agent is 4% of that of the pentane, and the volume of the crosslinking accelerator is 3.0% of that of the pentane, wherein the gelling agent is an oil-based fracturing fluid gelling agent with the mass content of 80% of dialkyl aluminum phosphate prepared by adding toluene into dialkyl aluminum phosphate in example 4 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof'.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 4.75s, and the fracturing fluid becomes jelly within 21.39 s; the viscosity was found to be 613.6 mPas.
Example 14
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 10g of potassium hydroxide, 5g of ferric sulfate with a mass content of 20%, 20mL of ethanol, 40mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing hydrocarbons prepared by using the crosslinking accelerator comprises a base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is propane, the volume of the gelling agent is 3% of that of the propane, the volume of the crosslinking accelerator is 3.0% of that of the propane, the gelling agent is an oil-based fracturing fluid gelling agent with the patent number of ZL00100278.3 and the mass content of dialkyl aluminum phosphate prepared by adding toluene into dialkyl aluminum phosphate in example 2 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof' is 80%.
Putting the fracturing fluid into a closed pressure container with a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears in 4.69s, and the fracturing fluid becomes jelly in 21.06 s; the viscosity was 621.7 mPas, as measured with a D100/200 system.
Example 15
In the crosslinking accelerator for the anhydrous fracturing of hydrocarbon of this embodiment, each 100mL of the crosslinking accelerator contains 3g of potassium hydroxide, 5g of ferric sulfate with a mass content of 20%, 20mL of ethanol, 40mL of ethylene glycol, and the balance of water; and uniformly mixing the substances to obtain the crosslinking accelerator for the hydrocarbon anhydrous fracturing fluid.
The anhydrous fracturing fluid containing carbon hydrocarbons prepared by using the crosslinking accelerator comprises a base fluid, a gelling agent and the crosslinking accelerator, wherein the base fluid is hexane, the volume of the gelling agent is 5% of that of the hexane, and the volume of the crosslinking accelerator is 3.0% of that of the hexane, wherein the gelling agent is an oil-based fracturing fluid gelling agent with the mass content of 80% of dialkyl aluminum phosphate prepared by adding toluene into dialkyl aluminum phosphate in example 2 disclosed in the invention patent of 'an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof'.
Putting the fracturing fluid into a magnetic stirrer, starting the magnetic stirrer and simultaneously pressing a stopwatch, wherein the vortex disappears within 5.60s, and the fracturing fluid becomes jelly within 23.56 s; the viscosity was found to be 667.9 mPas.
Example 16
In this example, the carbon hydrocarbon anhydrous fracturing fluid corresponding to example 5 was used, the gel formed after gelling was placed in a beaker, sodium acetate was added as a gel breaker, and after stirring, the gel breaker was heated in a water bath at 80 ℃ to form a gel breaker solution, wherein the amount of the gel breaker was 0.8g per 100mL of the carbon hydrocarbon anhydrous fracturing fluid.
In the present example, the time taken for forming the gel breaking solution was 2.5 hours, and the gel was restored to the state before gelling.
Example 17
In this example, the carbon hydrocarbon anhydrous fracturing fluid corresponding to example 5 was used, the gel formed after gelling was placed in a beaker, sodium acetate was added as a gel breaker, and after stirring, the gel breaker was heated in a water bath at 80 ℃ to form a gel breaker solution, wherein the amount of the gel breaker was 2.0g per 100mL of the carbon hydrocarbon anhydrous fracturing fluid.
In this example, the time taken for forming the gel breaking solution was 1 hour, the gel recovered to a clear and bright state before gelation, and the precipitate at the bottom of the beaker was completely dissolved by stirring.
Example 18
In this example, the carbon hydrocarbon anhydrous fracturing fluid corresponding to example 12 was used, the gel formed after gelling was placed in a beaker, sodium acetate was added as a gel breaker, the mixture was stirred uniformly and then heated in a water bath at 80 ℃ to form a gel breaker solution, wherein the amount of the gel breaker was 2.4g per 100mL of the carbon hydrocarbon anhydrous fracturing fluid.
In this example, the time taken for forming the gel breaking solution was 3 hours, and the gel was restored to the state before gelation.
Example 19
In this example, the gel breaking solution corresponding to example 16 was used, and a re-gelling accelerator and a gelling agent were added to the gel breaking solution, wherein the volume of the re-gelling accelerator was 7% of the volume of the gel breaking solution, and the volume of the gelling agent was 0.5% of the volume of the gel breaking solution, and the re-gelling accelerator was a mixed solution of absolute ethanol and concentrated sulfuric acid having a mass concentration of 98.3% mixed in a volume ratio of 9:0.5, and the gelling agent was ZL00100278.3, which was an oil-based fracturing fluid gelling agent prepared by adding toluene to dialkyl aluminum phosphate of example 3 disclosed in the invention patent of "an aluminum phosphate oil-based fracturing fluid gelling agent and a method for preparing the same", and had a mass content of dialkyl aluminum phosphate of 40%.
Example 20
In this example, the gel breaking solution corresponding to example 17 was used, and a re-gelling accelerator and a gelling agent were added to the gel breaking solution, wherein the volume of the re-gelling accelerator was 9% of the volume of the gel breaking solution, and the volume of the gelling agent was 1% of the volume of the gel breaking solution, and the re-gelling accelerator was a mixed solution of absolute ethanol and concentrated sulfuric acid having a mass concentration of 98.3% in a volume ratio of 9:1, and the gelling agent was an oil-based fracturing fluid gelling agent having a mass content of 80% of dialkyl aluminum phosphate prepared by adding toluene to dialkyl aluminum phosphate of example 3 disclosed in the invention patent of "an aluminum phosphate oil-based fracturing fluid gelling agent and a method for preparing the same".
Example 21
In this example, the gel breaking solution corresponding to example 18 is adopted, and a re-gelling accelerator and a gelling agent are added to the gel breaking solution, wherein the volume of the re-gelling accelerator is 11% of the volume of the gel breaking solution, the volume of the gelling agent is 2% of the volume of the gel breaking solution, the secondary utilization fracturing fluid is formed after uniform stirring, the re-gelling accelerator is a mixed solution of absolute ethyl alcohol and concentrated sulfuric acid with the mass concentration of 98.3% in a volume ratio of 9:1.5, and the gelling agent is an oil-based fracturing fluid gelling agent with the mass content of 50% of dialkyl aluminum phosphate prepared by adding toluene to dialkyl aluminum phosphate in example 3 disclosed in the invention patent with the patent number of ZL00100278.3 and the name of "an aluminum phosphate oil-based fracturing fluid gelling agent and a preparation method thereof".
The gelling time, viscosity and temperature resistance of the hydrocarbon anhydrous fracturing fluids of example 19, example 20 and example 21 were examined. The gelling time is determined by a stopwatch, the fracturing fluid is placed in a magnetic stirrer, the stopwatch is pressed while the magnetic stirrer is started, and the time required for vortex disappearance and the time required for the fracturing fluid to become gel are respectively recorded; the viscosity of the fracturing fluid was measured by a Hakke rotational viscometer. The results are shown in Table 4.
Table 4 examples 19-21 gel formation times and viscosities for secondary use fracturing fluids
From table 4, the viscosity of the secondary utilization fracturing fluid formed by adding the gelling agent and the re-gelling accelerator after the gel breaking of the hydrocarbon anhydrous fracturing fluid of the invention is maintained at a high level.
From FIG. 5, at 170s-1At a shear rate of 40 ℃ to 120 ℃ and a secondary use fracturing fluid (example 20) viscosity of about 200 mPas. As can be seen from fig. 2 and 5, the temperature resistance of the secondary utilization fracturing fluid can reach the temperature resistance level before gel breaking.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (4)
1. A crosslinking accelerator for a carbon-hydrocarbon anhydrous fracturing fluid is characterized in that each 100mL of the crosslinking accelerator contains 5g of sodium hydroxide, 1g of ferric sulfate, 20mL of ethanol, 40mL of ethylene glycol and the balance of water.
2. A hydrocarbon-based anhydrous fracturing fluid prepared by using the crosslinking accelerator of claim 1, which comprises a base fluid, a gelling agent and a crosslinking accelerator, wherein the volume of the gelling agent is 3 to 5 percent of the volume of the base fluid, and the volume of the crosslinking accelerator is 1 to 3 percent of the volume of the base fluid, and the gelling agent is the gelling agent disclosed in the invention patent No. ZL00100278.3 entitled "aluminum phosphate oil-based fracturing fluid gelling agent and preparation method thereof"; the base liquid is diesel oil, crude oil, kerosene, hexane, pentane or propane; after the carbon hydrocarbon anhydrous fracturing fluid is gelled, the gel breaking fluid is broken by a gel breaker to form a gel breaking fluid, and the gel breaking fluid is mixed with the gelling agent and a secondary gelling accelerator to be secondarily utilized as the fracturing fluid; the volume of the gelatinizing agent is 0.5-2% of the volume of the gel breaking liquid, the volume of the re-gelatinizing accelerant is 7-11% of the volume of the gel breaking liquid, and the re-gelatinizing accelerant is a mixed solution of absolute ethyl alcohol and concentrated sulfuric acid with the mass concentration of 98.3% according to the volume ratio of 9 (0.5-1.5).
3. The hydrocarbon-based anhydrous fracturing fluid of claim 2, wherein the volume of the gelling agent in the hydrocarbon-based anhydrous fracturing fluid is 4% of the volume of the base fluid, and the volume of the crosslinking promoter is 2.4% of the volume of the base fluid.
4. The anhydrous hydrocarbon fracturing fluid of claim 2, wherein the gel breaker is sodium acetate, and the amount of the gel breaker is 0.8-2.4 g per 100mL of the anhydrous hydrocarbon fracturing fluid.
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| CN104498017A (en) * | 2014-12-22 | 2015-04-08 | 中国石油天然气股份有限公司 | Fracturing fluid cross-linking agent and preparation method and application thereof |
| CN105176510A (en) * | 2015-09-06 | 2015-12-23 | 四川省贝特石油技术有限公司 | Preparation method of fracturing fluid for anhydrous organic temporary plugging turnaround fracturing |
| CN107446564A (en) * | 2016-05-30 | 2017-12-08 | 中国石油化工股份有限公司 | A kind of lower carbon number hydrocarbons fracturing fluid crosslinking agent and preparation method |
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| US6544934B2 (en) * | 2001-02-23 | 2003-04-08 | Halliburton Energy Services, Inc. | Methods and compositions for treating subterranean formations with gelled hydrocarbon fluids |
| US9518212B2 (en) * | 2005-08-08 | 2016-12-13 | Ethox Chemicals, Llc | Low volatile phosphorous gelling agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104498017A (en) * | 2014-12-22 | 2015-04-08 | 中国石油天然气股份有限公司 | Fracturing fluid cross-linking agent and preparation method and application thereof |
| CN105176510A (en) * | 2015-09-06 | 2015-12-23 | 四川省贝特石油技术有限公司 | Preparation method of fracturing fluid for anhydrous organic temporary plugging turnaround fracturing |
| CN107446564A (en) * | 2016-05-30 | 2017-12-08 | 中国石油化工股份有限公司 | A kind of lower carbon number hydrocarbons fracturing fluid crosslinking agent and preparation method |
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