CN113499732B - Fracturing fluid and preparation method and application thereof - Google Patents
Fracturing fluid and preparation method and application thereof Download PDFInfo
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- CN113499732B CN113499732B CN202110776335.2A CN202110776335A CN113499732B CN 113499732 B CN113499732 B CN 113499732B CN 202110776335 A CN202110776335 A CN 202110776335A CN 113499732 B CN113499732 B CN 113499732B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C07—ORGANIC CHEMISTRY
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- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/02—Acyclic radicals, not substituted by cyclic structures
- C07H15/04—Acyclic radicals, not substituted by cyclic structures attached to an oxygen atom of the saccharide radical
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/30—Viscoelastic surfactants [VES]
Abstract
The invention discloses a fracturing fluid and a preparation method and application thereof, and belongs to the technical field of coal seam water injection. The fracturing fluid comprises a surfactant, a nano material and a clay stabilizer; the nano-composite material is obtained by uniformly mixing a surfactant, a nano material, a clay stabilizer and water at 50 ℃. The fracturing fluid can be well immersed into a coal body to interact with the coal body, so that the wettability of the coal body is increased, a surfactant in the fracturing fluid plays a role of a bridge between coal molecules and water molecules, on one hand, a hydrophobic group is combined with the coal molecules, on the other hand, the water molecules are dragged, and the surface tension of water is effectively reduced, so that the water immersion amount into the coal body during coal seam water injection is increased, the coal dust yield in the subsequent coal mining process is reduced, and the safety production of a coal mine and the body health of operators are guaranteed.
Description
Technical Field
The invention relates to the technical field of coal seam water injection, in particular to a fracturing fluid and a preparation method and application thereof.
Background
The coal industry is always used as an important energy structure support in China, plays an important role in the rise of new China and the development of the economic society, and still occupies a major position in future energy structures in China along with the rapid development of science and technology and the continuous maturation of the new coal industry. The coal mine underground dust hazard is a technical problem to be solved in the development process of the coal mine industry. The comprehensive mechanized coal mining face (called fully mechanized coal mining face for short) is used as the place with the largest dust output of the coal mine, the dust output of the comprehensive mechanized coal mining face accounts for about 60% of the dust output of the coal mine, and the comprehensive mechanized coal mining face is the key point of dust prevention and dust fall. Under the condition that no measures are taken in some coal mines, the dust concentration of the fully mechanized coal mining face can reach 5000- 3 Even in the moment of fully mechanized coal mining, the original dust concentration is even as high as 8000mg/m 3 The operation environment is seriously polluted, the physical health of coal miners is influenced, and high-concentration dust easily causes dust explosion accidents, thereby causing huge threat to the life and health of underground operators.
Theoretically, coal seam water injection is a fundamental measure for dust prevention and dust fall of a fully mechanized coal mining face. However, most coal bodies in coal mines have the problems of hard coal quality, few original pore fractures, poor hydrophilicity and the like, belong to coal seams which are difficult to inject water, and the purposes of reducing critical pressure, increasing the wetting radius of water injection, expanding water injection area and improving water storage speed are difficult to achieve by using water only, so that the coal seam water injection needs to adopt fracturing fluid. There are many types of fracturing fluids in use today, with water-based fracturing fluids and oil-based fracturing fluids being used more widely. However, a potential problem with water-based fracturing fluids is that they can cause severe damage to subterranean reservoirs. Oil-based fracturing fluids generally consist of hydrocarbons (crude oil and diesel oil) and gel breakers (strong base and weak acid salts), but due to the influence of the crude oil and other substances, the fracturing fluids generally have the problems of high cost, poor shear resistance, large fluid loss and the like. And the two types of fracturing fluids have poor effect with coal bodies, have small influence on the dust yield during coal mining, and cannot play a role in preventing dust and reducing dust fundamentally.
Therefore, the technical problems to be solved urgently at present are to improve the performance defects of the traditional fracturing fluid, improve the water injection and moistening softening capacity of the coal bed, reduce the yield of coal dust during coal mining and ensure the safety production of the coal mine and the physical health of operating personnel.
Disclosure of Invention
The invention aims to provide a fracturing fluid and a preparation method and application thereof, so as to solve the problems in the prior art, improve the performance defects of the traditional fracturing fluid, improve the water injection and wetting softening capabilities of a coal seam, reduce the yield of coal dust during coal mining, and ensure the safe production of a coal mine and the body health of operators.
In order to achieve the purpose, the invention provides the following scheme:
one of the purposes of the invention is to provide a surfactant, wherein the surfactant is a compound shown as a formula I and a formula II, or a mixture consisting of the formula I and the formula II;
the invention also aims to provide a preparation method of the surfactant, which comprises the following steps:
step 1, preparing an intermediate product: lauryl glucoside and benzoic acid are catalyzed by ferrous sulfate to obtain an intermediate product;
the intermediate product is a compound shown in a formula III or a formula IV or a mixture composed of the formula III and the formula IV;
step 2, preparing a surfactant: and reacting the intermediate product with amidopropyl dimethylamine oleate under an acidic condition to obtain the surfactant.
Further, in the step 1, the benzoic acid is one or two of p-benzoic acid and s-tribenzoic acid.
Further, the acidic condition in step 2 is hydrochloric acid, sulfuric acid or nitric acid.
Further, the reaction process of step 1 is as follows:
reaction process of trimesic acid and lauryl glucoside:
reaction process of terephthalic acid and lauryl glucoside:
reaction procedure of mixture of trimesic acid and terephthalic acid with lauryl glucoside:
further, the reaction process of step 2 is as follows:
intermediate product of the reaction of trimesic acid with lauryl glucoside preparation of surfactants:
preparation of surfactant from intermediate of reaction of terephthalic acid with lauryl glucoside:
preparation of surfactant from a mixture of trimesic acid and terephthalic acid with lauryl glucoside reaction intermediate:
the invention also aims to provide the application of the surfactant in the fracturing fluid.
The fourth purpose of the invention is to provide a fracturing fluid, which comprises a surfactant, a nano material and a clay stabilizer;
the surfactant is the surfactant.
Further, the water-based nano-material coating comprises, by mass, 2.84-4.26 wt% of a surfactant, 0.75-1.43wt% of a nano material, 1.93-2.72 wt% of a clay stabilizer and the balance of water. The nano material is one or two of nano titanium dioxide or nano silicon dioxide; the clay stabilizer is one or two of sodium chloride or potassium chloride.
The fifth purpose of the invention is to provide a preparation method of the fracturing fluid, which is to uniformly mix a surfactant, a nano material, a clay stabilizer and water;
the temperature of the mixing was 50 ℃.
The invention further aims to provide the application of the fracturing fluid in coal seam water injection.
The mechanism of the invention is as follows:
under the action of ferrous sulfate, activating carboxyl on lauryl glucoside by an active ester method to perform esterification reaction with carboxyl on trimesic acid to prepare an intermediate product, polymerizing oleamidopropyl dimethylamine on the intermediate product in a branched chain form by amidation reaction with oleamidopropyl dimethylamine under the conditions of acidity, sealing and organic solvent to obtain a surfactant compound, wherein the synthesized surfactant has more obvious hydrophilic groups (carboxyl groups and hydroxyl groups) and two hydrophobic carbon chains, and under the condition of adding water, the nano titanium dioxide can promote the interaction of the hydrophilic groups and the hydrophobic groups to form rod-shaped or worm-shaped micelles with stronger viscosity, and the amide groups and ester groups generated in the reaction ensure that the fracturing fluid has certain adhesion to a coal bed and can reduce filtration loss in the fracturing process, the hydroxyl and carboxyl groups enhance the wetting of the resulting overall structure to the coal seam. And the added clay stabilizer can prevent the water-sensitive minerals from hydration expansion and dispersion migration, can play a role in increasing the wetting, improves the permeability of the coal bed and provides convenience for the next coal bed wetting.
The invention discloses the following technical effects:
(1) the fracturing fluid can be well immersed into a coal body to interact with the coal body, so that the wettability of the coal body is improved, the fracturing fluid mainly plays a role of a bridge between coal molecules and water molecules due to the existence of surfactant molecules in the fracturing fluid, one side of the fracturing fluid is combined with the coal molecules by virtue of a similar compatibility mechanism, and the other side of the fracturing fluid is used for drawing the water molecules by virtue of acting forces such as hydrogen bonds and the like, so that the surface tension of water is effectively reduced, the water immersion amount of the coal body during coal seam water injection is increased, the water storage amount of the coal body is increased in a subsequent water injection process, and the yield of coal dust in a subsequent coal mining process is further reduced;
(2) the invention meets the corresponding cleaning standard, has better shearing stability and lower filtration loss, has better wetting and softening performance on coal bodies, has good effect on reducing the yield of coal dust during coal mining, and ensures the safety production of coal mines and the health of operators.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the embodiments will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow diagram of the present invention for preparing a fracturing fluid;
FIG. 2 is a graph showing the results of uniaxial compression tests performed after the coal pillar test pieces were immersed in water and the fracturing fluids prepared in examples 1 to 3 for 24 hours, and then dried.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in that stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
Example 1
Step 1, preparing an intermediate product: adding lauryl glucoside and trimesic acid into water in a molar ratio of 1:1 in a three-neck flask with a thermometer and a stirring device, wherein the molar ratio of the water to the lauryl glucoside is 500:1, uniformly mixing, adding 0.5mol of ferrous sulfate as a catalyst, carrying out ultrasonic treatment for 1h, fully mixing, and carrying out N-phase ultrasonic treatment on the mixture 2 Reacting at 95 ℃ for 3h under protection, then transferring into petroleum ether, washing, filtering and drying to obtain light yellow powder-an intermediate product (formula III);
the reaction process is as follows:
step 2, preparing a surfactant: the intermediate product is prepared by mixing the following components in a molar ratio: amidopropyl dimethylamine oleate: adding hydrochloric acid at a ratio of 1:1:1 into an ethyl acetate aqueous solution with a molar ratio of 1:1, wherein the molar ratio of the intermediate product to ethyl acetate is 1:10, uniformly mixing, sealing, reacting at 85 ℃ for 18h, adding a proper amount of potassium hydroxide to adjust the pH to 6-7, finally carrying out reduced pressure distillation to remove ethyl acetate, carrying out recrystallization by using propylene oxide, and removing unreacted oleamide propyl dimethylamine to obtain the surfactant (formula I);
the reaction process is as follows:
step 3, preparing a fracturing fluid: uniformly mixing 2.84 wt% of surfactant, 1.43wt% of nano titanium dioxide, 1.93 wt% of sodium chloride and the balance of water at 50 ℃ to prepare fracturing fluid (marked as Z1).
Example 2
Step 1, preparing an intermediate product: adding lauryl glucoside, trimesic acid and p-benzoic acid into water in a molar ratio of 2:1:1 in a three-neck flask with a thermometer and a stirring device, wherein the molar ratio of the water to the lauryl glucoside is 500:1, uniformly mixing, adding 0.5mol of ferrous sulfate as a catalyst, carrying out ultrasonic treatment for 1 hour, fully mixing, and then carrying out N-phase ultrasonic treatment on the mixture 2 Reacting at 95 ℃ for 3h under protection, then transferring into petroleum ether, washing, filtering and drying to obtain light yellow powder, namely an intermediate product (a mixture of a formula III and a formula IV);
the reaction process is as follows:
step 2, preparing a surfactant: the intermediate product is prepared by mixing the following components in a molar ratio: oleamide propyl dimethylamine: adding hydrochloric acid at a ratio of 1:1:1 to an ethyl acetate aqueous solution with a molar ratio of 1:1, wherein the molar ratio of the intermediate product to the ethyl acetate is 1:10, uniformly mixing, sealing, reacting at 85 ℃ for 18h, adding a proper amount of potassium hydroxide to adjust the pH to 6-7, finally performing reduced pressure distillation to remove the ethyl acetate, performing recrystallization by using propylene oxide, and removing unreacted oleamidopropyl dimethylamine to obtain a surfactant (a mixture of formula I and formula II);
the reaction process is as follows:
step 3, preparing a fracturing fluid: and uniformly mixing 3.5 wt% of a surfactant product, 1.2 wt% of nano silicon dioxide, 2.3 wt% of potassium chloride and the balance of water at the temperature of 50 ℃ to prepare the fracturing fluid (marked as Z2).
Example 3
Step 1, preparing an intermediate product: adding lauryl glucoside and terephthalic acid into water in a molar ratio of 1:1 in a three-neck flask with a thermometer and a stirring device, wherein the molar ratio of the water to the lauryl glucoside is 500:1, uniformly mixing, adding 0.5mol of ferrous sulfate as a catalyst, performing ultrasonic treatment for 1h, fully mixing, and performing ultrasonic treatment on the mixture in N 2 Reacting at 95 ℃ for 3h under protection, then transferring into petroleum ether, washing, filtering and drying to obtain light yellow powder-an intermediate product (formula IV);
the reaction process is as follows:
step 2, preparing a surfactant: and (3) mixing the intermediate product: amidopropyl dimethylamine oleate: adding hydrochloric acid at a ratio of 1:1:1 into an ethyl acetate aqueous solution with a molar ratio of 1:1, wherein the molar ratio of the intermediate product to ethyl acetate is 1:10, uniformly mixing, sealing, reacting at 85 ℃ for 18h, adding a proper amount of potassium hydroxide to adjust the pH to 6-7, finally carrying out reduced pressure distillation to remove ethyl acetate, carrying out recrystallization by using propylene oxide, and removing unreacted oleamide propyl dimethylamine to obtain a surfactant (formula II);
the reaction process is as follows:
step 3, preparing a fracturing fluid: and uniformly mixing 4.26 wt% of a surfactant product, 0.75 wt% of a mixture of nano titanium dioxide and nano silicon dioxide in a mass ratio of 1:1, 1.43wt% of a mixture of sodium chloride and potassium chloride in a mass ratio of 1:1 and the balance of water at the temperature of 50 ℃ to prepare the fracturing fluid (marked as Z3).
I Performance evaluation of fracturing fluids Z1, Z2 and Z3 prepared in examples 1 to 3
The fracturing fluid belongs to a viscoelastic surfactant fracturing system, and the technical standard of the fracturing fluid adopts a method for evaluating the performance of water-based fracturing fluid, which is shown in Table 4 (general technical index of viscoelastic surfactant fracturing fluid) in SY/T6376-2008 'general technical conditions for fracturing fluid', and SY/5107-.
1. Shear viscosity
The apparent viscosity and shear stability of the fracturing fluid were evaluated using a model ZNN-D12 digital viscometer. Table 1 shows the fracturing fluid at 170s -1 The change in apparent viscosity at shear rate of 30min, as can be seen at 170s -1 Shearing for 30min at a shearing rate, wherein the apparent viscosity of each fracturing fluid is about 300 mPas, which shows that the fracturing fluid prepared by the method has better shearing stability.
TABLE 1 apparent viscosity of fracturing fluids
2. Fluid loss property
The fluid loss of the fracturing fluid was evaluated using a high temperature and high pressure fluid loss instrument. The fluid loss coefficient and the initial fluid loss of the fracturing fluid are calculated through a high-temperature high-pressure fluid loss instrument in the following calculation mode:
wherein: c-filtration loss coefficient controlled by Filter cake, m/min 1/2 (ii) a Slope of the m-fluid loss curve, ml/min 1/2 (ii) a A-area of fluid loss, cm 2 (ii) a v is initial filtration loss, m/min; h-intercept, cm, of the straight line segment of the fluid loss curve with the y-axis 2 。
As shown in table 2, it is understood from table 2 that the fluid loss of the fracturing fluid is small and meets the required standards of the fracturing fluid.
TABLE 2 fluid loss properties of fracturing fluids
| Item | Z1 | Z2 | Z3 | General technical standard |
| Coefficient of fluid loss (m/min) 1/2 ) | 0.84×10 -3 | 0.87×10 -3 | 0.96×10 -3 | 1.0×10 -3 |
| Initial fluid loss (m) 3 /m 2 ) | 0.033 | 0.042 | 0.044 | 0.05 |
3. Wettability of
As shown in table 3, the results of the contact angle test, in which the wettability of the fracturing fluid was evaluated and compared with the contact angle of water, show that the contact angle of the briquette after the action of the fracturing fluid was small and the wetting effect was excellent in table 3.
TABLE 3 wettability of fracturing fluids
4. Softening property
Firstly, prepared coal pillar test pieces (with the diameter of 50mm and the height of 100mm) are respectively placed in water, Z1, Z2 and Z3 for soaking for 24 hours, then the coal pillar test pieces are dried and then subjected to a uniaxial compression experiment, and the experimental result is shown in figure 2.
The coal column test piece (diameter is 50mm, height is 100mm) is prepared and is respectively placed in water, Z1, Z2 and Z3 to be soaked for 24h, then the water absorption performance test (the weight difference of the test piece is verified after the test piece is soaked for different time), the coal dust yield test after fracturing (the dust yield is determined by cutting coal after wetting) is carried out on the coal column test piece, the experimental results are shown in Table 4, the experimental results show that the coal column test piece soaked in the fracturing fluid has better water absorption performance, and the coal dust yield test results after fracturing show that the coal column test piece treated by the fracturing fluid generates less coal dust and has the effect of reducing the coal dust.
TABLE 4 analysis of fracturing fluid data on water absorption and dust production rates of coal samples
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (8)
1. The surfactant is characterized in that the surfactant is a compound shown in a formula I or a formula II, or a mixture of the formula I and the formula II;
2. the method of claim 1, comprising the steps of:
step 1, preparing an intermediate product: lauryl glucoside and benzoic acid are catalyzed by ferrous sulfate to obtain an intermediate product;
the intermediate product is a compound shown in a formula III or a formula IV or a mixture composed of the formula III and the formula IV;
step 2, preparing a surfactant: and reacting the intermediate product with oleamide propyl dimethylamine under an acidic condition, and removing impurities and recrystallizing to obtain the surfactant.
3. The method for preparing a surfactant according to claim 2, wherein the benzoic acid in step 1 is one or both of terephthalic acid and trimesic acid.
4. Use of the surfactant of claim 1 in a fracturing fluid.
5. The fracturing fluid is characterized by comprising a surfactant, a nano material and a clay stabilizer;
the surfactant is the surfactant of claim 1.
6. The fracturing fluid of claim 5, wherein the fracturing fluid comprises, by mass, 2.84-4.26% of a surfactant, 0.75-1.43% of a nanomaterial, 1.93-2.72% of a clay stabilizer, and the balance of water; the nano material is one or two of nano titanium dioxide or nano silicon dioxide; the clay stabilizer is one or two of sodium chloride or potassium chloride.
7. The method for preparing the fracturing fluid according to claim 5 or 6, wherein the fracturing fluid is obtained by uniformly mixing the surfactant, the nano material, the clay stabilizer and water;
the temperature of the mixing was 50 ℃.
8. Use of a fracturing fluid according to claim 5 or 6 in the injection of water into a coal seam.
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