Petroleum fracturing propping agent containing fly ash component and preparation method thereof
By performing high-temperature treatment and component optimization on fly ash, petroleum fracturing proppants with a tight network structure are formed, which solves the problem of material bonding defects in the prior art and improves the strength and crushing rate performance of the proppant.
Patent Information
- Application Number
- CN202510915470.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-03
- Publication Date
- 2025-08-01
- Estimated Expiration
- 2045-07-03
AI Technical Summary
During the preparation process, the existing petroleum fracturing proppants have defects in the combination of various components, which affects strength performance.
Fly ash is used as the base material, and after magnetic separation, flotation, screening and high-temperature calcination, dimethyl sulfoxide, sodium hexametaphosphate, nanosilica and nanozirconia are combined to form a tight three-dimensional network structure, optimize the surface structure and interface combination, and spray-dry it into spherical particles to improve strength performance.
It improves the compressive strength and crushing rate performance of petroleum fracturing proppants, enhances the stability and density of the material, and reduces the crushing caused by local stress concentration.
Smart Images

Figure CN120399671A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of fracturing proppants, and specifically to a petroleum fracturing proppant containing fly ash components and a preparation method thereof. Background Art
[0002] Petroleum fracturing proppants are key materials in fracturing operations for unconventional oil and gas exploitation such as shale gas. They are carried into formation fractures by fracturing fluid, and their function is to support the fractures to remain open, ensuring the smooth flow of oil and gas to the wellbore, which is crucial for improving oil and gas production and development efficiency.
[0003] In the prior art, petroleum fracturing proppants are prepared by mixing and sintering various high-hardness materials. After preparation, there are problems with defects in the combination of each component material, which affects the strength performance of the petroleum fracturing proppants. Based on this, the present invention provides a petroleum fracturing proppant containing fly ash components and a preparation method thereof. Summary of the Invention
[0004] The purpose of the present invention is to provide a petroleum fracturing proppant containing fly ash components and a preparation method thereof. The petroleum fracturing proppant prepared by the present invention not only has good compressive strength performance but also has excellent breakage rate performance, effectively improving the service performance of the petroleum fracturing proppant.
[0005] To achieve the above purpose, the present invention provides the following technical solutions: In the first aspect, the present invention provides a petroleum fracturing proppant containing fly ash components, which comprises the following raw material components: zircon sand, quartz sand, clay, sodium hexametaphosphate, powder, bauxite powder, binder. The weight percentages of each raw material are: 8 - 10% quartz sand, 1 - 2% clay, 2 - 4% sodium hexametaphosphate, 12 - 16% powder, 1 - 2% bauxite powder, 4 - 6% binder, and the balance is made up to 100% by zircon sand; The preparation of the powder comprises the following steps: S1: Preparation of the base material, and fly ash is selected as the raw material of the base material; S2: Preparation of the mixture, and the raw materials of the mixture include dimethyl sulfoxide, diethylenetriaminepentaacetic acid, 3-aminopropylmethyldimethoxysilane, methyl ethylene glycol chitosan, N-hydroxysuccinimide, polyvinylpyrrolidone, deionized water; S3: Mixing treatment, the base material and the mixture are subjected to mixing treatment to obtain the powder.
[0006] Further, the method for preparing the base material is as follows: fly ash is treated by magnetic separation and flotation to remove impurities, and then subjected to screening treatment. The particle size of the fly ash after screening is 200-300 μm. The screened fly ash is added into a muffle furnace for calcination treatment. The set heating rate for the calcination treatment is 10-20 °C / min, and the temperature is raised to 800-900 °C and kept warm for 30-50 min. After the calcination treatment is completed, it is waited to cool to room temperature. The obtained product is added into a mixer, and a sodium hydroxide solution is added into the mixer. The mixer is set to stir at 400-600 r / min for 30-40 min. The obtained product is washed with deionized water, and then subjected to filtration and drying treatments to prepare the base material.
[0007] Further, the mass of the sodium hydroxide solution is 2-3 times the mass of the fly ash after screening, and the mass concentration of the sodium hydroxide solution is 4-6%.
[0008] Further, the method for preparing the mixture is as follows: dimethyl sulfoxide is added into a water bath pot, and the water bath is heated to 70-80 °C. Then diethylenetriaminepentaacetic acid is added. The water bath pot is connected to a magnetic stirrer, and the magnetic stirrer is set to rotate at 80-120 r / min for constant-temperature stirring treatment for 10-20 min. Then the temperature is set to be raised to 100-120 °C, and 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, and N-hydroxysuccinimide are added for constant-temperature reaction for 20-30 min. After cooling to 70-80 °C, polyvinylpyrrolidone is added, the temperature is set to 60-70 °C, and the rotation speed of the magnetic stirrer is 100-200 r / min for constant-temperature stirring treatment for 2-4 h. The obtained product and deionized water are added into a mixer, and the mixer is set to stir at 400-600 r / min for 20-30 min to prepare the mixture.
[0009] Further, the mass ratio of the raw materials in the mixture is 100:(4-6):(6-8):(10-12):(2-4):(0.8-1.2):(200-220).
[0010] Further, the mass ratio of the base material to the mixture is 1:(1.6-1.8).
[0011] Further, the method of the mixing treatment is as follows: The base material and the mixture are added into a mixer, and the mixer is set to stir at 400 - 600 r / min for 30 - 40 min to obtain a slurry. The slurry is pumped into a spray drying tower for spray granulation treatment. The spray drying tower is set with an inlet temperature of 160 - 180 °C, an outlet temperature of 80 - 90 °C, an atomization pressure of 0.3 - 0.5 MPa, and a feeding rate of 10 - 20 L / h to obtain granular materials. The granular materials, nano-silica, and nano-zirconia are added into a mixer, and the mixer is set to stir at 600 - 800 r / min for 40 - 50 min to complete the mixing treatment and obtain powder materials.
[0012] Further, the particle sizes of the nano-silica and the nano-zirconia are 10 - 30 nm, the mass of the nano-silica is 5 - 7% of the mass of the granular materials, and the mass of the nano-zirconia is 1 - 3% of the mass of the granular materials.
[0013] Further, the binder selected is silica sol.
[0014] In the second aspect, the present invention also provides a preparation method of a petroleum fracturing proppant containing fly ash components, including the following steps: Weigh zircon sand, quartz sand, clay, sodium hexametaphosphate, powder materials, bauxite powder, and binder as required and add them into a mixer. The mixer is set to stir at 600 - 800 r / min for 40 - 50 min to obtain a mixture. The mixture is added into a disk granulator for granulation treatment, and the granulation particle size is 150 - 200 μm. The obtained product is subjected to sintering treatment. The heating rate is set to 5 - 10 °C / min, heated to 300 - 500 °C, and held for 20 - 30 min. Then the heating rate is set to 10 - 20 °C / min, heated to 1200 - 1300 °C, and held for 20 - 30 min to obtain the petroleum fracturing proppant.
[0015] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. In the present invention, in the preparation of the petroleum fracturing proppant, after the fly ash undergoes high-temperature and alkali treatment, its surface structure can be optimized. As a polar solvent, dimethyl sulfoxide can assist in the uniform dispersion of each component. 3-aminopropylmethyldimethoxysilane can improve the interfacial bonding between the fly ash and other component materials and enhance the adhesion between the particulate materials. Diethylenetriaminepentaacetic acid and N-hydroxysuccinimide can synergistically chelate metal ions to form a tight three-dimensional network structure and enhance the stability of each structural combination in the petroleum fracturing proppant, thereby achieving the purpose of improving the strength performance of the petroleum fracturing proppant.
[0016] 2. In the present invention, the addition of nano-silica and nano-zirconia can play a role in filling micropores in the oil fracturing proppant system. After filling the micropores, it can inhibit grain coarsening, achieve the purpose of refining the grain size after sintering and improving the material density. Through the combined spray drying treatment of the base material and the mixture, uniform spherical particles are formed after spray drying. These spherical particles can evenly distribute stress during the use of the fracturing proppant, reduce the breakage caused by local stress concentration, and further improve the strength performance of the oil fracturing proppant. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 FIG. is a flowchart of a petroleum fracturing proppant containing fly ash components and a preparation method thereof proposed by the invention. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0018] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0019] Among them, it should be noted that the raw materials used in the following embodiments are all commercially available raw materials.
[0020] Example 1:
[0021] Raw material preparation: 8% quartz sand, 1% clay, 2% sodium hexametaphosphate, 12% powder, 1% bauxite powder, 4% binder, and the balance is made up to 100% with zircon sand; The preparation of the powder includes the following steps: S1: Preparation of the base material, and fly ash is selected as the raw material of the base material; The method for preparing the base material is as follows: Fly ash is treated by magnetic separation and flotation to remove impurities, and then screened. The particle size of the fly ash after screening is 200 μm. The screened fly ash is added to a muffle furnace for calcination. The set heating rate for the calcination treatment is 10 °C / min, and the temperature is raised to 800 °C and held for 30 min. After the calcination treatment is completed, wait for it to cool to room temperature. The obtained product is added to a mixer, and sodium hydroxide solution is added to the mixer. The mixer is set to stir at 400 r / min for 30 min. The obtained product is washed with deionized water, and then filtered and dried to obtain the base material. Among them, the mass of the sodium hydroxide solution is 2 times the mass of the fly ash after screening, and the mass concentration of the sodium hydroxide solution is 4%; S2: Preparation of the mixture. The raw materials of the mixture include dimethyl sulfoxide, diethylenetriaminepentaacetic acid, 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, N-hydroxysuccinimide, polyvinylpyrrolidone, and deionized water. The method for preparing the mixture is as follows: Dimethyl sulfoxide is added to a water bath pot, and the water bath is heated to 70°C. Then, diethylenetriaminepentaacetic acid is added. The water bath pot is connected to a magnetic stirrer, and the magnetic stirrer is set at a rotation speed of 80 r / min for constant-temperature stirring for 10 min. Then, the temperature is set to rise to 100°C, and 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, and N-hydroxysuccinimide are added for constant-temperature reaction for 20 min. After cooling to 70°C, polyvinylpyrrolidone is added, the temperature is set to 60°C, and the magnetic stirrer rotation speed is 100 r / min for constant-temperature stirring for 2 h. The obtained product and deionized water are added to a mixer, and the mixer is set to stir at 400 r / min for 20 min to prepare the mixture. Among them, the mass ratio of each raw material in the mixture is 100:4:6:10:2:0.8:200, and the mass ratio of the base material to the mixture is 1:1.6. S3: Mixing treatment. The base material and the mixture are subjected to mixing treatment to obtain a powder material. The method for mixing treatment is as follows: The base material and the mixture are added to a mixer, and the mixer is set to stir at 400 r / min for 30 min to obtain a slurry. The slurry is pumped into a spray drying tower for spray granulation treatment. The spray drying tower is set with an inlet temperature of 160°C, an outlet temperature of 80°C, an atomization pressure of 0.3 MPa, and a feeding rate of 10 L / h to obtain granular materials. The granular materials, nano-silica, and nano-zirconia are added to a mixer, and the mixer is set to stir at 600 r / min for 40 min to complete the mixing treatment and obtain a powder material.
[0022] The particle sizes of nano-silica and nano-zirconia are 10 nm. The mass of nano-silica is 5% of the mass of the granular materials, and the mass of nano-zirconia is 1% of the mass of the granular materials.
[0023] The binder is selected as silica sol.
[0024] Preparation of petroleum fracturing proppants: It includes the following steps: Weigh zircon sand, quartz sand, clay, sodium hexametaphosphate, powder material, bauxite powder, and binder as needed and add them to a mixer. The mixer is set to stir at 600 r / min for 40 min to obtain a mixed material. The mixed material is added to a disk granulator for granulation treatment, and the granulation particle size is 150 μm. The obtained product is subjected to sintering treatment. The heating rate is set to 5°C / min and heated to 300°C, then kept warm for 20 min. Then, the heating rate is set to 10°C / min and heated to 1200°C, and kept warm for 20 min to obtain petroleum fracturing proppants.
[0025] Example Two:
[0026] Raw material preparation: 9% quartz sand, 1.5% clay, 3% sodium hexametaphosphate, 14% powder, 1.5% bauxite powder, 5% binder, and the balance is made up to 100% with zircon sand; The preparation of the powder includes the following steps: S1: Preparation of the base material. The raw material of the base material is fly ash. The method for preparing the base material is as follows: Fly ash is treated by magnetic separation and flotation to remove impurities, and then screened. The particle size of the fly ash after screening is 250 μm. The screened fly ash is added to a muffle furnace for calcination. The set heating rate for the calcination treatment is 15 °C / min, and it is heated to 850 °C and kept warm for 40 min. After the calcination treatment is completed, it is waited to cool to room temperature. The obtained product is added to a mixer, and sodium hydroxide solution is added to the mixer. The mixer is set to stir at 500 r / min for 35 min. The obtained product is washed with deionized water, and then filtered and dried to obtain the base material. Among them, the mass of the sodium hydroxide solution is 2.5 times the mass of the fly ash after screening, and the mass concentration of the sodium hydroxide solution is 5%; S2: Preparation of the mixture. The raw materials of the mixture include dimethyl sulfoxide, diethylenetriaminepentaacetic acid, 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, N-hydroxysuccinimide, polyvinylpyrrolidone, and deionized water; The method for preparing the mixture is as follows: Dimethyl sulfoxide is added to a water bath pot, and the water bath is heated to 75 °C. Then diethylenetriaminepentaacetic acid is added. The water bath pot is connected to a magnetic stirrer, and the magnetic stirrer is set to rotate at 100 r / min for constant-temperature stirring for 15 min. Then it is set to heat up to 110 °C, and 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, and N-hydroxysuccinimide are added for constant-temperature reaction for 25 min. After cooling to 75 °C, polyvinylpyrrolidone is added, the temperature is set to 65 °C, and the magnetic stirrer rotates at 150 r / min for constant-temperature stirring for 3 h. The obtained product and deionized water are added to a mixer, and the mixer is set to stir at 500 r / min for 25 min to obtain the mixture. Among them, the mass ratio of each raw material in the mixture is 100:5:7:11:3:1:210, and the mass ratio of the base material to the mixture is 1:1.7; S3: Mixing treatment. The base material and the mixture are subjected to mixing treatment to obtain the powder; The method of mixing treatment is as follows: The base material and the mixing agent are added into a mixer. The mixer is set to stir at 500 r / min for 35 min to obtain a slurry. The slurry is pumped into a spray drying tower for spray granulation treatment. The spray drying tower is set with an inlet temperature of 170 °C, an outlet temperature of 85 °C, an atomization pressure of 0.4 MPa, and a feeding rate of 15 L / h to obtain granular materials. The granular materials, nano-silica, and nano-zirconia are added into a mixer. The mixer is set to stir at 700 r / min for 45 min to complete the mixing treatment and obtain powder materials.
[0027] The particle sizes of nano-silica and nano-zirconia are 20 nm. The mass of nano-silica is 6% of the mass of the granular materials, and the mass of nano-zirconia is 2% of the mass of the granular materials.
[0028] The binder is selected as silica sol.
[0029] Preparation of petroleum fracturing proppants: It includes the following steps: Weigh zircon sand, quartz sand, clay, sodium hexametaphosphate, powder materials, bauxite powder, and binder as required and add them into a mixer. The mixer is set to stir at 700 r / min for 45 min to obtain a mixed material. The mixed material is added into a disk granulator for granulation treatment. The granule size of granulation is 170 μm. The obtained product is subjected to sintering treatment. The heating rate is set to 7 °C / min and heated to 400 °C, and kept warm for 25 min. Then the heating rate is set to 15 °C / min and heated to 1250 °C, and kept warm for 25 min to obtain petroleum fracturing proppants.
[0030] Example 3:
[0031] Raw material preparation: 10% quartz sand, 2% clay, 4% sodium hexametaphosphate, 16% powder materials, 2% bauxite powder, 6% binder, and the balance is supplemented with zircon sand to 100%; The preparation of the powder materials includes the following steps: S1: Preparation of the base material. The raw material of the base material is selected as fly ash. The method for preparing the base material is as follows: Fly ash is treated by magnetic separation and flotation to remove impurities, and then subjected to screening treatment. The particle size of the fly ash after screening is 300 μm. The screened fly ash is added into a muffle furnace for calcination treatment. The heating rate of the calcination treatment is set to 20 °C / min and heated to 900 °C, and kept warm for 50 min. After the calcination treatment is completed, wait for it to cool to room temperature. The obtained product is added into a mixer, and sodium hydroxide solution is added into the mixer. The mixer is set to stir at 600 r / min for 40 min. The obtained product is washed with deionized water, and then subjected to filtration and drying treatment to obtain the base material. Among them, the mass of the sodium hydroxide solution is 3 times the mass of the screened fly ash, and the mass concentration of the sodium hydroxide solution is 6%; S2: Preparation of the mixture. The raw materials of the mixture include dimethyl sulfoxide, diethylenetriaminepentaacetic acid, 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, N-hydroxysuccinimide, polyvinylpyrrolidone, and deionized water. The method for preparing the mixture is as follows: Dimethyl sulfoxide is added to a water bath pot, and the water bath is heated to 80°C. Then, diethylenetriaminepentaacetic acid is added. The water bath pot is connected to a magnetic stirrer, and the magnetic stirrer is set at a rotation speed of 120 r / min for constant-temperature stirring for 20 min. Then, the temperature is set to rise to 120°C, and 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, and N-hydroxysuccinimide are added for constant-temperature reaction for 30 min. After cooling to 80°C, polyvinylpyrrolidone is added, the temperature is set to 70°C, and the rotation speed of the magnetic stirrer is 200 r / min for constant-temperature stirring for 4 h. The obtained product and deionized water are added to a mixer, and the mixer is set at 600 r / min for stirring for 30 min to obtain the mixture. Among them, the mass ratio of each raw material in the mixture is 100:6:8:12:4:1.2:220, and the mass ratio of the base material to the mixture is 1:1.8. S3: Mixing treatment. The base material and the mixture are subjected to mixing treatment to obtain the powder material. The method for mixing treatment is as follows: The base material and the mixture are added to a mixer, and the mixer is set at 600 r / min for stirring for 40 min to obtain the slurry. The slurry is pumped into a spray drying tower for spray granulation treatment. The inlet temperature of the spray drying tower is set at 180°C, the outlet temperature is 90°C, the atomization pressure is 0.5 MPa, and the feeding rate is 20 L / h to obtain the granular material. The granular material, nano-silica, and nano-zirconia are added to a mixer, and the mixer is set at 800 r / min for stirring for 50 min to complete the mixing treatment and obtain the powder material.
[0032] The particle sizes of nano-silica and nano-zirconia are 30 nm. The mass of nano-silica is 7% of the mass of the granular material, and the mass of nano-zirconia is 3% of the mass of the granular material.
[0033] The binder is selected as silica sol.
[0034] Preparation of petroleum fracturing proppants: It includes the following steps: Weigh zircon sand, quartz sand, clay, sodium hexametaphosphate, powder material, bauxite powder, and binder as required and add them to a mixer. The mixer is set at 800 r / min for stirring for 50 min to obtain the mixture. The mixture is added to a disk granulator for granulation treatment. The granulation particle size is 200 μm. The obtained product is subjected to sintering treatment. The heating rate is set at 10°C / min and heated to 500°C, and kept warm for 30 min. Then, the heating rate is set at 20°C / min and heated to 1300°C, and kept warm for 30 min to obtain the petroleum fracturing proppants.
[0035] Comparative Example 1. The difference between this comparative example and Example 1 is that this comparative example does not contain diethylenetriaminepentaacetic acid.
[0036] Comparative Example 2. The difference between this comparative example and Example 1 is that this comparative example does not contain nano-silica and nano-zirconia.
[0037] Comparative Example 3. The difference between this comparative example and Example 1 is that this comparative example uses an equal amount of fly ash to replace the powder material.
[0038] Comparative Example 4. The difference between this comparative example and Example 1 is that this comparative example does not contain powder material.
[0039] Performance test: Perform performance tests on the petroleum fracturing proppants prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4. The obtained test data are recorded in the following table:
[0040] In the performance test, adopt the test method in GB / T17431-2019 to conduct compressive strength performance tests on the petroleum fracturing proppants prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4; Adopt the test method in SY / T5108-2014 to conduct breakage rate performance tests on the petroleum fracturing proppants prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4.
[0041] It can be seen that the strength performance of the petroleum fracturing proppants prepared in Comparative Examples 1, 2, 3, and 4 is lower than that in Examples 1, 2, and 3. This shows that: in the preparation of petroleum fracturing proppants, after fly ash is treated at high temperature and with alkali, its surface structure can be optimized. Dimethyl sulfoxide, as a polar solvent, can assist in the uniform dispersion of each component. 3-aminopropylmethyldimethoxysilane can improve the interfacial bonding between fly ash and other component materials and enhance the adhesion between granular materials. Diethylenetriaminepentaacetic acid and N-hydroxysuccinimide can synergistically chelate metal ions to form a tight three-dimensional network structure, enhancing the stability of each structural combination in the petroleum fracturing proppant, thereby achieving the purpose of improving the strength performance of the petroleum fracturing proppant; The addition of nano-silica and nano-zirconia can play a role in filling micropores in the petroleum fracturing proppant system. After filling the micropores, it can play a role in inhibiting grain coarsening, achieving the purpose of refining the grain size after sintering and improving the material density. Through the combined spray drying treatment of the base material and the mixture, uniform spherical particles are formed after spray drying. The spherical particles can evenly distribute stress during the use of the fracturing proppant, reduce the breakage caused by local stress concentration, and further improve the strength performance of the petroleum fracturing proppant.
[0042] By comparing and analyzing the relevant data in the table, it can be seen that the petroleum fracturing proppant prepared by the present invention not only has good compressive strength performance, but also has excellent crushing rate performance. This shows that the petroleum fracturing proppant containing fly ash provided by the present invention has a broader market prospect and is more suitable for popularization.
[0043] In the description of this specification, the description with reference to terms such as "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.
[0044] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not elaborate all the details, nor do they limit the invention to the specific embodiments described. Obviously, many modifications and variations can be made according to the content of this specification. These embodiments are selected and specifically described in this specification in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and utilize the present invention well. The present invention is only limited by the claims and their full scope and equivalents.
Claims
1. An oil fracturing proppant containing fly ash components, characterized in that: It consists of the following raw materials: zircon sand, quartz sand, clay, sodium hexametaphosphate, powder material, bauxite powder, and binder. The weight percentages of each raw material are: 8 - 10% quartz sand, 1 - 2% clay, 2 - 4% sodium hexametaphosphate, 12 - 16% powder material, 1 - 2% bauxite powder, 4 - 6% binder, and the balance is made up to 100% with zircon sand; The preparation of the powder material includes the following steps: S1: Preparation of the base material. The raw material of the base material is fly ash; S2: Preparation of the mixture. The raw materials of the mixture include dimethyl sulfoxide, diethylenetriaminepentaacetic acid, 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, N-hydroxysuccinimide, polyvinylpyrrolidone, and deionized water; S3: Mixing treatment. The base material and the mixture are subjected to mixing treatment to obtain the powder material.
2. The petroleum fracturing proppant containing fly ash component according to claim 1, characterized in that, The method for preparing the base material is as follows: Fly ash is treated by magnetic separation and flotation to remove impurities, and then subjected to screening treatment. The particle size of the fly ash after screening is 200 - 300 μm. The screened fly ash is added to a muffle furnace for calcination treatment. The set heating rate for the calcination treatment is 10 - 20 °C / min, and it is heated to 800 - 900 °C and held for 30 - 50 min. After the calcination treatment is completed, it is allowed to cool to room temperature. The obtained product is added to a mixer, and a sodium hydroxide solution is added to the mixer. The mixer is set to stir at 400 - 600 r / min for 30 - 40 min. The obtained product is washed with deionized water, and then filtered and dried to obtain the base material.
3. The petroleum fracturing proppant containing fly ash component according to claim 2, wherein The mass of the sodium hydroxide solution is 2 - 3 times the mass of the fly ash after screening, and the mass concentration of the sodium hydroxide solution is 4 - 6%.
4. The petroleum fracturing proppant containing fly ash component according to claim 1, characterized in that, The method for preparing the mixture is as follows: Dimethyl sulfoxide is added to a water bath pot, and the water bath is heated to 70 - 80 °C. Then diethylenetriaminepentaacetic acid is added. The water bath pot is connected to a magnetic stirrer, and the magnetic stirrer is set to rotate at 80 - 120 r / min for constant-temperature stirring treatment for 10 - 20 min. Then it is set to be heated to 100 - 120 °C, and 3-aminopropylmethyldimethoxysilane, methyl glycol chitosan, and N-hydroxysuccinimide are added for constant-temperature reaction for 20 - 30 min. After cooling to 70 - 80 °C, polyvinylpyrrolidone is added, and the temperature is set to 60 - 70 °C, and the rotation speed of the magnetic stirrer is 100 - 200 r / min for constant-temperature stirring treatment for 2 - 4 h. The obtained product and deionized water are added to a mixer, and the mixer is set to stir at 400 - 600 r / min for 20 - 30 min to obtain the mixture.
5. The oil fracturing proppant containing fly ash component according to claim 1, characterized in that, The mass ratio of each raw material in the mixture is 100:(4 - 6):(6 - 8):(10 - 12):(2 - 4):(0.8 - 1.2):(200 - 220).
6. The petroleum fracturing proppant containing fly ash component according to claim 1, characterized in that The mass ratio of the base material to the mixture is 1:(1.6 - 1.8).
7. The petroleum fracturing proppant containing fly ash component according to claim 1, characterized in that The method of the mixing treatment is as follows: The base material and the mixture are added into a mixer. The mixer is set to stir at 400 - 600 r / min for 30 - 40 min to obtain a slurry. The slurry is pumped into a spray drying tower for spray granulation treatment. The spray drying tower is set with an inlet temperature of 160 - 180 °C, an outlet temperature of 80 - 90 °C, an atomization pressure of 0.3 - 0.5 MPa, and a feeding rate of 10 - 20 L / h to obtain granular materials. The granular materials, nano-silica, and nano-zirconia are added into a mixer. The mixer is set to stir at 600 - 800 r / min for 40 - 50 min to complete the mixing treatment and obtain powder materials.
8. The petroleum fracturing proppant containing fly ash component according to claim 7, characterized in that, The particle sizes of nano-silica and nano-zirconia are 10 - 30 nm. The mass of nano-silica is 5 - 7% of the mass of the granular materials, and the mass of nano-zirconia is 1 - 3% of the mass of the granular materials.
9. The petroleum fracturing proppant containing fly ash component according to claim 1, wherein The binder selected is silica sol.
10. A preparation method of a petroleum fracturing proppant containing fly ash component according to claim 1, characterized in that, It includes the following steps: Weigh zircon sand, quartz sand, clay, sodium hexametaphosphate, powder materials, bauxite powder, and binder as required and add them into a mixer. The mixer is set to stir at 600 - 800 r / min for 40 - 50 min to obtain a mixture. The mixture is added into a disk granulator for granulation treatment. The granule size of granulation is 150 - 200 μm. The obtained product is subjected to sintering treatment. The heating rate is set to 5 - 10 °C / min and heated to 300 - 500 °C, and kept warm for 20 - 30 min. Then the heating rate is set to 10 - 20 °C / min and heated to 1200 - 1300 °C, and kept warm for 20 - 30 min to obtain petroleum fracturing proppants.
Citation Information
Patent Citations
Petroleum fracturing propping agent containing fly ash in raw materials and preparation method thereof
CN103497757A
Method for coproducing petroleum fracturing proppant and xonotlite by using high-alumina fly ash
CN106867502A
Low-density and high-strength ceramsite proppant prepared by utilizing bauxite tailings and fly ash
CN108706960A
Preparation method and application of magnetic cellulose microspheres with core-shell structure
CN110681361A
Dry powder polymer online mixing and fracturing method for oil and gas field
CN119145828A