CN113430669B - Synthesis method and application of temperature-resistant, salt-resistant and shear-resistant fiber material for fracturing fluid - Google Patents

Synthesis method and application of temperature-resistant, salt-resistant and shear-resistant fiber material for fracturing fluid Download PDF

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CN113430669B
CN113430669B CN202110496487.7A CN202110496487A CN113430669B CN 113430669 B CN113430669 B CN 113430669B CN 202110496487 A CN202110496487 A CN 202110496487A CN 113430669 B CN113430669 B CN 113430669B
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fracturing fluid
temperature
polyamide resin
shear
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姚海雷
刘飞
刘清雪
代晓东
李聪聪
李雷
张昕
张小杰
刘清源
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Shengli College China University of Petroleum
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    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/78Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/80Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • C08G69/34Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids using polymerised unsaturated fatty acids
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/62Compositions for forming crevices or fractures
    • C09K8/66Compositions based on water or polar solvents
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/80Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
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    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
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    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
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    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/356Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides

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Abstract

The invention relates to the technical field of synthetic reaction process methods of polyamide fiber materials, in particular to a synthetic method and application of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid. The technical scheme is as follows: the method comprises the following steps: according to 1.6 percent of the weight of the dimer acid feed, slowly adding diamine, and stirring at a constant speed; slowly adding an acid additive according to 1.6 percent of the weight of the dimer acid feed, and stirring at a constant speed; according to 11 percent of the weight of the dimer acid fed in each time, dripping ethylenediamine, and stirring at a constant speed; gradually raising the temperature of the reaction kettle to 180 ℃ while dropwise adding the ethylenediamine, keeping the temperature for 1 hour, raising the temperature to 235 ℃, and reacting for 3-4 hours at the temperature; dehydrating to obtain the polyamide resin product. The beneficial effects are that: the polyamide resin produced by the method has the characteristics of environmental protection, low production cost and the like, has good dispersibility and compatibility in water-based fracturing fluid, and can be uniformly dispersed in the fracturing fluid; the temperature resistance, salt tolerance and shear resistance of the fracturing fluid are improved.

Description

Synthesis method and application of temperature-resistant, salt-resistant and shear-resistant fiber material for fracturing fluid
Technical Field
The invention relates to the technical field of synthetic reaction process methods of polyamide fiber materials, in particular to a synthetic method and application of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid.
Background
At present, China has become the first energy consuming country in the world, and the demand of China for energy will be further expanded in the coming years according to the current development situation. In recent years, the demand of petroleum in China increases at a rate of about 6% per year, and in contrast, the yield of crude oil in China is increased by less than 2% per year, so that a great part of crude oil needs to be imported from abroad. According to prediction, the import quantity of crude oil needs to be increased by more than 10 percent, the import quantity of finished oil needs to be increased by more than 8 percent and the dependency of oil import exceeds 70 percent in the coming years, so that the economic development of China is greatly influenced and the stable and rapid development of economy is severely restricted. Therefore, increasing crude oil production in our country has become a priority in recent years in the petroleum industry. China has abundant oil reserves, but geology and exploitation conditions are not ideal, most oil reservoirs belong to three-low (low-permeability, low-pressure and low-abundance) oil reservoirs, the quantity of petroleum which can be exploited nationwide exceeds 200 hundred million tons, the low-permeability reserves account for up to 66 percent, and the ultra-low-permeability and ultra-low-permeability oil reservoirs account for more than half. Therefore, how to develop the low permeability reservoir and increase the petroleum yield of the low permeability reservoir has important significance on the sustainable development of oil and gas resources in China.
The fracturing technique is an oil and gas stimulation that uses pressure to fracture the formation and propped the fracture with a proppant to reduce the flow resistance of the oil and gas. The key core of the research and development of the fracturing technology is the development of fracturing fluid, and the performance of the fracturing fluid plays a decisive role in the success of the fracturing yield increase process of the oil and gas field. At present, the fracturing fluids which are applied more mainly comprise vegetable gum fracturing fluids, cellulose derivative fracturing fluids and synthetic polymer fracturing fluids, but the traditional fracturing fluids have the defects of poor temperature resistance and salt tolerance, weak shear resistance, large damage to the stratum, high cost and the like, so that a novel fracturing fluid which is good in temperature resistance and salt tolerance, strong in shear resistance, small damage to the stratum and low in cost is urgently needed in an oil-gas field. After the fibers are added into the traditional polyacrylamide fracturing fluid, the fibers and polyacrylamide molecular chains form a winding structure together, and the strength of a cross-linked reticular structure is enhanced, so that the temperature resistance, salt tolerance, shear resistance, sand carrying capacity and the like of the fracturing fluid are improved, and the fracturing yield-increasing effect of an oil-gas field can be effectively improved.
Disclosure of Invention
The invention aims to provide a synthesis method and application of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid aiming at the defects in the prior art, the polyamide resin produced by the method can be used as a raw material of fiber in a novel fiber fracturing fluid, and has the characteristics of environmental protection, low production cost and the like, and the prepared modified chopped polyamide resin fiber has good dispersibility and compatibility in a water-based fracturing fluid and can be uniformly dispersed in the fracturing fluid; the modified short-cut polyamide resin fiber with a certain amount is added into the traditional polymer fracturing fluid, so that the concentration of the polymer required in the traditional fracturing fluid can be obviously reduced, the temperature resistance, salt tolerance and shear resistance of the fracturing fluid are improved, a good fracturing yield-increasing effect is finally realized, and the economic benefit and the environmental benefit of the fracturing operation of an oil-gas field are obviously improved.
The invention provides a method for synthesizing a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid, which adopts the technical scheme that: the method comprises the following steps:
firstly, cleaning a reaction kettle until the reaction kettle is dry, clean and free of impurities, and checking that feeding pipelines and discharging pipelines are smooth;
secondly, starting a liquid feeding pipeline of the reaction kettle, adding dimer acid, closing the feeding pipeline, stirring for 30 minutes, and sampling to test viscosity;
thirdly, slowly adding diamine according to 1.6 percent of the weight of the fed dimer acid every time, and uniformly stirring by a stirrer in the kettle in the process;
step four, slowly adding the acid additive according to 1.6 percent of the weight of the dimer acid fed in each time, and stirring at a constant speed by a stirrer in the kettle in the process;
fifthly, starting an ethylene diamine feeding pipeline, dropwise adding ethylene diamine according to 11% of the weight of the dimer acid fed each time, wherein the amine adding time is about 40 minutes, and in the process, a stirrer in the kettle is used for stirring at a constant speed;
step six, gradually raising the temperature of the reaction kettle to 180 ℃ while dropwise adding the ethylenediamine, keeping the temperature for 1 hour after the temperature is raised to 180 ℃, raising the temperature to 235 ℃, and reacting for 3-4 hours at the temperature;
seventhly, after the sample in the reaction kettle is qualified in test, vacuumizing for 2 hours to complete the dehydration process, and then discharging to obtain a polyamide resin product;
eighthly, adding filler consisting of fumed silica, active calcium carbonate and titanium dioxide and polyamide resin into a high-speed mixer, blending at 360 ℃, and mixing at a shear rate of 2.5/s for 30-45 minutes;
ninth, extruding, spinning, solidifying and forming fibers at 260 ℃, cutting, washing and cooling to obtain the product with the density of 1.15g/cm3And a short-cut polyamide resin fiber having a diameter of 50 to 100 μm and a length of 6 to 9 mm.
Preferably, the dimer acid used in the above is a dimer acid having a viscosity of 5500 cP.
Preferably, the diamine is hexamethylenediamine, p-xylylenediamine or nonanediamine.
Preferably, the acidic auxiliary agent is glacial acetic acid, toluenesulfonic acid or benzenesulfonic acid.
The application of the temperature-resistant, salt-resistant and shear-resistant fiber material for the fracturing fluid comprises the following steps:
step ten, soaking the prepared chopped polyamide resin fibers by taking a PVP hydrophilic solution and a KH550 coupling agent solution as fiber treating agents to form a hydrophilic coating on the surfaces of the polyamide resin fibers;
and step eleven, adding the modified chopped polyamide resin fibers with the mass fraction of 0.0-0.6% into the traditional polyacrylamide fracturing fluid, and uniformly dispersing to obtain the temperature-resistant, salt-resistant and shear-resistant polyamide resin fiber fracturing fluid.
Compared with the prior art, the invention has the following beneficial effects:
1. aiming at the problems of high cost, serious pollution and difficult degradation of petrochemical raw materials, the invention adopts the plant-based dimer acid as the main raw material to synthesize the semi-plant-based polyamide resin fiber which is used for improving the temperature resistance, salt tolerance and shear resistance of the traditional polyacrylamide fracturing fluid, and the novel fiber fracturing fluid is green, environment-friendly and low in cost;
2. the invention aims to perform surface hydrophilic modification on polyamide resin fibers: the PVP hydrophilic solution and the KH550 coupling agent solution are used as polyamide resin fiber treating agents, the prepared polyamide resin fiber is subjected to surface hydrophilic modification treatment, and a hydrophilic coating is formed on the surface of the polyamide resin fiber, so that the dispersion effect of the polyamide resin fiber in the fracturing fluid is obviously improved;
3. the invention aims to add the prepared chopped polyamide resin fiber into the polyacrylamide fracturing fluid to: after a certain amount of modified chopped polyamide resin fibers are added into the polyacrylamide fracturing fluid, when the fibers are dispersed in the fracturing fluid, the fibers and polyacrylamide molecular chains form a winding structure together, the strength of a cross-linked reticular structure is enhanced, and the temperature resistance, salt tolerance and shear resistance of the fracturing fluid are improved;
through the measures, the invention can further reduce the production cost of the fracturing fluid and improve the oil-gas yield increasing effect in the fracturing process of the oil-gas field, and has good economic value and environmental significance.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1:
the invention provides a method for synthesizing a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid, which comprises the following steps:
3 tons of dimer acid with the viscosity of 5500cP are put into the reaction kettle and stirred for 30 minutes; under the condition of uniform stirring, slowly adding hexamethylene diamine accounting for 1.6 percent of the weight of the dimer acid feed;under the condition of uniform stirring, slowly adding glacial acetic acid accounting for 1.6 percent of the weight of the dimer acid feed; under the condition of uniform stirring, slowly adding ethylenediamine which accounts for 11 percent of the weight of the dimer acid feed, and controlling the amine adding time to be about 40 minutes; dropwise adding ethylenediamine, gradually raising the temperature of the reaction kettle to 180 ℃, keeping the temperature for 1 hour, raising the temperature to 235 ℃, and reacting for 3-4 hours; vacuumizing for 2 hours to complete the dehydration process to obtain a polyamide resin product; adding filler consisting of fumed silica, active calcium carbonate and titanium dioxide and polyamide resin into a high-speed mixer, and mixing at 360 ℃ for 30-45 minutes at a shear rate of 2.5/s; extruding, spinning, solidifying and forming fibers, cutting, washing and cooling at 260 ℃ to obtain the product with the density of 1.15g/cm3And a chopped polyamide resin fiber having a diameter of 50 to 100 μm and a length of 6 to 12 mm.
The invention relates to an application of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid, which comprises the following steps:
soaking the prepared chopped polyamide resin fiber by taking PVP hydrophilic solution and KH550 coupling agent solution as fiber treating agents to form a hydrophilic layer on the surface of the fiber; and then, adding 0.0-0.6 wt% of modified chopped polyamide resin fiber into the polyacrylamide fracturing fluid, and uniformly dispersing to obtain the temperature-resistant, salt-resistant and shear-resistant polyamide resin fiber fracturing fluid.
In addition, it should be noted that:
(1) the plant-based dimer acid is used as a main raw material and reacts with raw materials such as ethylenediamine, hexamethylenediamine, glacial acetic acid and the like to synthesize the semi-bio-based polyamide resin, the main raw material dimer acid of the semi-bio-based polyamide resin is mainly produced by using plant-based oleic acid such as soybean oleic acid, rapeseed oleic acid, tall oil acid and the like, and is a conventional commercially available product, so that the consumption of petrochemical products is remarkably reduced in the production process of the polyamide resin, the preparation process is green and pollution-free, and the generation cost is lower;
(2) the method comprises the following steps of taking semi-bio-based polyamide resin as a raw material, adopting a novel wire drawing/wire blowing process, and carrying out extrusion, spinning, solidification and fiber forming, cutting, water washing, cooling and the like to produce polyamide resin fibers; the polyamide resin fiber is innovatively subjected to surface hydrophilic modification treatment, so that the polyamide resin fiber has good dispersibility and compatibility in the fracturing fluid and can be uniformly dispersed in the fracturing fluid;
(3) the influences of factors such as the length and the addition amount of polyamide resin fibers on the temperature resistance, salt tolerance and shear resistance of the fracturing fluid are researched, the proper length and the addition amount of the polyamide resin fibers are preferably selected, and finally the novel polyamide resin fiber fracturing fluid with excellent temperature resistance, salt tolerance and shear resistance is prepared.
Example 2:
the invention provides a method for synthesizing a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid, which comprises the following steps:
3 tons of dimer acid with the viscosity of 5500cP are put into the reaction kettle and stirred for 30 minutes; slowly adding p-xylylenediamine accounting for 1.6 percent of the weight of the feed of the dimer acid under uniform stirring; slowly adding p-toluenesulfonic acid accounting for 1.6 percent of the weight of the dimer acid feed under uniform stirring; under the condition of uniform stirring, slowly adding ethylenediamine which accounts for 11 percent of the weight of the dimer acid feed, and controlling the amine adding time to be about 40 minutes; dropwise adding ethylenediamine, gradually raising the temperature of the reaction kettle to 180 ℃, keeping the temperature for 1 hour, raising the temperature to 235 ℃, and reacting for 3-4 hours; vacuumizing for 2 hours to complete the dehydration process to obtain a polyamide resin product; adding filler consisting of fumed silica, active calcium carbonate and titanium dioxide and polyamide resin into a high-speed mixer, and mixing at 360 ℃ for 30-45 minutes at a shear rate of 2.5/s; extruding, spinning, solidifying and forming fibers, cutting, washing and cooling at 260 ℃ to obtain the product with the density of 1.15g/cm3And a chopped polyamide resin fiber having a diameter of 50 to 100 μm and a length of 6 to 12 mm.
The invention relates to an application of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid, which comprises the following steps:
soaking the chopped polyamide resin fibers by taking PVP hydrophilic solution and KH550 coupling agent solution as fiber treating agents to form a hydrophilic layer on the surfaces of the chopped polyamide resin fibers; and adding 0.0-0.6 wt% of modified chopped polyamide resin fiber into the polyacrylamide fracturing fluid, and uniformly dispersing to obtain the temperature-resistant, salt-resistant and shear-resistant polyamide resin fiber fracturing fluid.
In addition, it should be noted that:
(1) the plant-based dimer acid is used as a main raw material and reacts with raw materials such as ethylenediamine, xylylenediamine, toluenesulfonic acid and the like to synthesize the semi-bio-based polyamide resin, the main raw material dimer acid of the semi-bio-based polyamide resin is mainly produced from plant-based oleic acid such as soybean oleic acid, rapeseed oleic acid, tall oil acid and the like, and is a conventional commercially available product, so that the consumption of petrochemical products is remarkably reduced in the production process of the polyamide resin, the preparation process is green and pollution-free, and the generation cost is lower;
(2) the method comprises the following steps of taking semi-bio-based polyamide resin as a raw material, adopting a novel wire drawing/wire blowing process, and carrying out extrusion, spinning, solidification and fiber forming, cutting, water washing, cooling and the like to produce polyamide resin fibers; the polyamide resin fiber is innovatively subjected to surface hydrophilic modification treatment, so that the polyamide resin fiber has good dispersibility and compatibility in the fracturing fluid and can be uniformly dispersed in the fracturing fluid;
(3) the influences of factors such as the length and the addition amount of polyamide resin fibers on the temperature resistance, salt tolerance and shear resistance of the fracturing fluid are researched, the proper length and the addition amount of the polyamide resin fibers are preferably selected, and finally the novel polyamide resin fiber fracturing fluid with excellent temperature resistance, salt tolerance and shear resistance is prepared.
Example 3:
the invention provides a synthesis method of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid, which comprises the following steps:
3 tons of dimer acid with the viscosity of 5500cP are put into a reaction kettle and stirred for 30 minutes; slowly adding 1,9 nonane diamine accounting for 1.6 percent of the weight of the dimer acid feed under uniform stirring; slowly adding benzenesulfonic acid accounting for 1.6 percent of the weight of the feed of the dimer acid under uniform stirring; under the condition of uniform stirring, slowly adding ethylenediamine which accounts for 11 percent of the weight of the dimer acid feed, and controlling the amine adding time to be about 40 minutes; dropwise adding ethylenediamine, gradually raising the temperature of the reaction kettle to 180 ℃, keeping the temperature for 1 hour, raising the temperature to 235 ℃, and reacting for 3-4 hours; vacuumizing for 2 hours to complete the dehydration process to obtain a polyamide resin product; the filler composed of fumed silica, active calcium carbonate and titanium dioxide is mixed with polyamideAdding the resin into a high-speed mixer, and mixing at 360 ℃ for 30-45 minutes at a shear rate of 2.5/s; extruding, spinning, solidifying and forming fibers, cutting, washing and cooling at 260 ℃ to obtain the product with the density of 1.15g/cm3And a chopped polyamide resin fiber having a diameter of 50 to 100 μm and a length of 6 to 12 mm.
The invention relates to an application of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid, which comprises the following steps:
soaking the chopped polyamide resin fibers by taking PVP hydrophilic solution and KH550 coupling agent solution as fiber treating agents to form a hydrophilic layer on the surfaces of the chopped polyamide resin fibers; and adding 0.0-0.6 wt% of modified chopped polyamide resin fiber into the polyacrylamide fracturing fluid, and uniformly dispersing to obtain the temperature-resistant, salt-resistant and shear-resistant polyamide resin fiber fracturing fluid.
In addition, it should be noted that:
(1) the plant-based dimer acid is used as a main raw material and reacts with raw materials such as ethylenediamine, nonanediamine, benzenesulfonic acid and the like to synthesize the semi-bio-based polyamide resin, the main raw material dimer acid of the semi-bio-based polyamide resin is mainly produced by using plant-based oleic acid such as soybean oleic acid, rapeseed oleic acid, tall oil acid and the like, and is a conventional commercially available product, so that the consumption of petrochemical products is remarkably reduced in the production process of the polyamide resin, the preparation process is green and pollution-free, and the generation cost is lower;
(2) the method comprises the following steps of taking semi-bio-based polyamide resin as a raw material, adopting a novel wire drawing/wire blowing process, and carrying out extrusion, spinning, solidification and fiber forming, cutting, water washing, cooling and the like to produce polyamide resin fibers; the polyamide resin fiber is innovatively subjected to surface hydrophilic modification treatment, so that the polyamide resin fiber has good dispersibility and compatibility in the fracturing fluid and can be uniformly dispersed in the fracturing fluid;
(3) the influences of factors such as the length and the addition amount of polyamide resin fibers on the temperature resistance, salt tolerance and shear resistance of the fracturing fluid are researched, the proper length and the addition amount of the polyamide resin fibers are preferably selected, and finally the novel polyamide resin fiber fracturing fluid with excellent temperature resistance, salt tolerance and shear resistance is prepared.
Example 4:
the preparation method of the polyamide resin fiber fracturing fluid comprises 0.8% of anionic polyacrylamide by mass, 0.01% of polysulfonate by mass, 25% of quartz sand (the particle size is 20 meshes) by volume and polyamide resin fibers (8 mm), DHE636, DXE636 and DNE636, wherein the mass ratio of the polyamide resin fibers to the quartz sand is 0.2%, and the balance is water. Referring to the petroleum and natural gas industry standard SY/T5107-1995 Water-based fracturing fluid evaluation method, the salinity is 3 percent and the shear rate is 170 s at 60 ℃ by using a rheometer-1Testing the shear stability of the fracturing fluid under the condition that the shear time is 120min to obtain that the viscosity of the sheared fiber fracturing fluid is 77 mPa & s, 60 mPa & s and 65 mPa & s respectively; under the same conditions, the viscosity of the fracturing fluid without the added fibers was 46 mPas after shearing.
TABLE 1 anti-shearing Properties of different types of Polyamide resin fiber fracturing fluids
Figure 484517DEST_PATH_IMAGE001
The experimental data in table 1 show that the fracturing fluid has low shear resistance and a test viscosity of 46 mPa · s when the polyamide resin fiber is not added; after 0.2% of polyamide resin fiber (8 mm) DHE636, DXE636 and DNE636 is added, the shearing resistance of the fracturing fluid is obviously improved; the effect of improving the shear resistance of the fracturing fluid is optimal by adding the polyamide resin fiber DHE636, and the viscosity can reach 87 mPa & s.
Example 5:
the polyamide resin fiber fracturing fluid comprises 0.8% by mass, 0.6% by mass, 0.4% by mass and 0.2% by mass of anionic polyacrylamide, 0.01% by mass of polysulfonate, 25% by volume of quartz sand (the particle size is 20 meshes) and polyamide resin fiber (8 mm) DHE636, wherein the mass ratios of the polyamide resin fiber to the quartz sand are respectively 0.0%, 0.2%, 0.4% and 0.6%, and the balance is water. Referring to the petroleum and natural gas industry standard SY/T5107-1995 evaluation method of water-based fracturing fluid, a rheometer is used at 60 ℃, the salinity is 3 percent, and the shear rate is 170 s-1Shear for cuttingAnd under the condition that the cutting time is 120min, testing the shear stability of the fracturing fluid to obtain that the viscosity of the fracturing fluid after shearing is 46 mPa & s, 77 mPa & s, 82 mPa & s and 70 mPa & s respectively.
TABLE 2 anti-shearing Properties of Polyamide resin fiber fracturing fluids
Figure 4360DEST_PATH_IMAGE002
The experimental data in Table 2 show that when the polyamide resin fiber DHE636 is not added, the anti-shearing capacity of the fracturing fluid is low, and the test viscosity is 46 mPa & s; after 0.2% -0.6% of polyamide resin fiber DHE636 is added, the shearing resistance of the fracturing fluid is obviously improved; the fracturing fluid of 0.4 percent of APAM and 0.4 percent of fiber (8 mm) has the best shearing resistance, and the viscosity can reach 83 mPa & s; experimental data show that the addition of polyamide resin fibers DHE636 into the fracturing fluid can significantly improve the shear resistance of the fracturing fluid, thereby significantly reducing the concentration of a thickening agent-polyacrylamide and realizing the reduction of the production cost of the fracturing fluid.
Example 6:
a polyamide resin fiber fracturing fluid comprises 0.4% of anionic polyacrylamide, 0.01% of polysulfonate, 25% of quartz sand (the particle size is 20 meshes) and polyamide resin fiber DHE636, wherein the fiber lengths are 6mm, 8mm, 10mm and 12mm respectively, the mass ratio of the polyamide resin fiber to the quartz sand is 0.4%, and the balance is water. Referring to the petroleum and natural gas industry standard SY/T5107-1995 evaluation method of water-based fracturing fluid, a rheometer is used at 60 ℃, the salinity is 3 percent, and the shear rate is 170 s-1And testing the shear stability of the fracturing fluid under the condition that the shear time is 120min to obtain that the viscosity of the fracturing fluid after shearing is 76mPa & s, 82 mPa & s and 94 mPa & s, 80 mPa & s respectively.
TABLE 3 influence of the fiber length of the polyamide resin on the fracturing fluid behavior
Figure 241569DEST_PATH_IMAGE003
The experimental data in the table 3 show that the addition of polyamide resin fiber DHE636 with the length of 6-12 mm into the fracturing fluid can improve the shear resistance of the fracturing fluid; and when the length of the polyamide resin fiber DHE636 is 10mm, the anti-shearing performance of the fracturing fluid is optimal, and the viscosity of the fracturing fluid after a shearing test reaches 94 mPa & s. The reason is that when the length of the fiber is smaller, the entanglement between the short fiber and the polyacrylamide molecular chain is weaker, but when the length of the fiber is too long, the fibers are tangled and agglomerated, so that the fibers form a uniform and loose dispersion system in the fracturing fluid and the shear stability of the fracturing fluid is not facilitated.
Example 7:
a polyamide resin fiber fracturing fluid comprises 0.4% by mass of anionic polyacrylamide, 0.01% by mass of polysulfonate, 25% by volume of quartz sand (the particle size is 20 meshes) and polyamide resin fiber DHE636 (10 mm), wherein the mass ratio of the polyamide resin fiber to the quartz sand is 0.4%, and the balance is water. Referring to SY/T5107 standard 1995 & ltWater-based fracturing fluid evaluation method & gt in petroleum and natural gas industry, a rheometer is used for respectively measuring the salinity of 3% and the shear rate of 170 s at different temperatures of 60 ℃, 90 ℃, 120 ℃ and 150 DEG C-1And testing the shear stability of the fracturing fluid under the condition that the shear time is 120min to obtain that the viscosity of the fracturing fluid after shearing is 94 mPa & s, 87 mPa & s, 80 mPa & s and 74 mPa & s respectively.
TABLE 4 temperature resistance of the polyamide resin fiber fracturing fluid
Figure 188665DEST_PATH_IMAGE004
From the experimental data in table 4, it can be seen that the viscosity of the fiber fracturing fluid after the shear test is gradually reduced with the increase of the temperature, but even when the temperature is increased to 150 ℃, the viscosity of the fracturing fluid after the shear test is still 74 mPa · s, which indicates that the fiber fracturing fluid can be used in a wider temperature range and has good temperature resistance.
Example 8:
the polyamide resin fiber fracturing fluid comprises the following components in percentage by mass0.4 percent of anionic polyacrylamide, 0.01 percent of polysulfonate, 25 percent of quartz sand (the particle size is 20 meshes) and polyamide resin fiber (10 mm), wherein the mass ratio of the polyamide resin fiber to the quartz sand is 0.4 percent, and the balance is water. Referring to the evaluation method of water-based fracturing fluid 1995 of SY/T5107--1And testing the shear stability of the fracturing fluid under the condition that the shear time is 120min to obtain that the viscosity of the fracturing fluid after shearing is respectively 98 mPa & s, 94 mPa & s, 87 mPa & s and 76mPa & s.
TABLE 5 salt resistance of Polyamide resin fiber fracturing fluids
Figure 78867DEST_PATH_IMAGE005
From the experimental data in table 5, it can be seen that the viscosity of the fiber fracturing fluid after the shear test is gradually reduced as the salinity is increased, but even if the salinity is up to 7%, the viscosity of the fracturing fluid after the shear test is still 76mPa · s, which indicates that the fiber fracturing fluid can be used in a wide salinity range and has good salt tolerance.
The above description is only a few preferred embodiments of the present invention, and any person skilled in the art may modify the above-described embodiments or modify them into equivalent ones. Therefore, any simple modifications or equivalent substitutions made in accordance with the technical solution of the present invention are within the scope of the claims of the present invention.

Claims (3)

1. A synthetic method of a temperature-resistant, salt-resistant and shear-resistant fiber material for a fracturing fluid is characterized by comprising the following steps: the method comprises the following steps:
firstly, cleaning a reaction kettle until the reaction kettle is dry, clean and free of impurities, and checking that feeding pipelines and discharging pipelines are smooth;
secondly, starting a liquid feeding pipeline of the reaction kettle, adding dimer acid, closing the feeding pipeline, stirring for 30 minutes, and sampling to test viscosity;
thirdly, slowly adding diamine according to 1.6 percent of the weight of the fed dimer acid every time, and uniformly stirring by a stirrer in the kettle in the process;
step four, slowly adding the acid additive according to 1.6 percent of the weight of the dimer acid fed in each time, and stirring at a constant speed by a stirrer in the kettle in the process;
fifthly, starting an ethylene diamine feeding pipeline, dropwise adding ethylene diamine according to 11% of the weight of the dimer acid fed each time, wherein the amine adding time is 40 minutes, and in the process, a stirrer in the kettle is used for stirring at a constant speed;
step six, gradually raising the temperature of the reaction kettle to 180 ℃ while dropwise adding the ethylenediamine, keeping the temperature for 1 hour after the temperature is raised to 180 ℃, raising the temperature to 235 ℃, and reacting for 3-4 hours at the temperature;
seventhly, after the sample in the reaction kettle is qualified in test, vacuumizing for 2 hours to complete the dehydration process, and then discharging to obtain a polyamide resin product;
eighthly, adding filler consisting of fumed silica, active calcium carbonate and titanium dioxide and polyamide resin into a high-speed mixer, blending at 360 ℃, and mixing at a shear rate of 2.5/s for 30-45 minutes;
ninth, extruding, spinning, solidifying and forming fibers at 260 ℃, cutting, washing and cooling to obtain the product with the density of 1.15g/cm3A short-cut polyamide resin fiber having a diameter of 50 to 100 μm and a length of 6 to 9 mm;
the dimer acid with the viscosity of 5500cP is adopted;
the diamine adopts hexamethylene diamine, p-xylylenediamine or nonane diamine.
2. The method for synthesizing the temperature, salt and shear resistant fiber material for the fracturing fluid as claimed in claim 1, which is characterized by comprising the following steps: the acidic auxiliary agent adopts glacial acetic acid, toluenesulfonic acid or benzenesulfonic acid.
3. The application of the temperature-resistant, salt-resistant and shear-resistant fiber material for the fracturing fluid prepared by the synthesis method according to claim 1 is characterized in that: the method comprises the following steps:
step ten, soaking the prepared chopped polyamide resin fibers by taking a PVP hydrophilic solution and a KH550 coupling agent solution as fiber treating agents to form a hydrophilic coating on the surfaces of the polyamide resin fibers;
and step eleven, adding the modified chopped polyamide resin fibers with the mass fraction of 0.0-0.6% into the traditional polyacrylamide fracturing fluid, and uniformly dispersing to obtain the temperature-resistant, salt-resistant and shear-resistant polyamide resin fiber fracturing fluid.
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