CN112080271A - Nickel-iron slag-based petroleum fracturing propping agent and preparation method thereof - Google Patents
Nickel-iron slag-based petroleum fracturing propping agent and preparation method thereof Download PDFInfo
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- CN112080271A CN112080271A CN202010937401.5A CN202010937401A CN112080271A CN 112080271 A CN112080271 A CN 112080271A CN 202010937401 A CN202010937401 A CN 202010937401A CN 112080271 A CN112080271 A CN 112080271A
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- 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
- 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
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
Abstract
The invention relates to the technical field of petroleum fracturing propping agents, in particular to a nickel-iron slag-based petroleum fracturing propping agent and a preparation method thereof, wherein the nickel-iron slag-based petroleum fracturing propping agent is prepared by the following steps: step one, uniformly mixing required amounts of a binder, a diluent, a curing agent and powder to obtain a mixed material, wherein the weight ratio of the binder to the diluent to the curing agent to the powder is 2.5-8.0: 1: 1: 15. the ferronickel slag-based petroleum fracturing propping agent is obtained by performing multistage shaping on ferronickel slag and then modifying the ferronickel slag and mixed materials. The proppant has good sphericity, low volume weight and good compressive strength, can meet the use requirements of the oil fracturing proppant, simultaneously realizes resource utilization of solid wastes, and effectively solves the problems that the natural quartz sand for fracturing of the existing oil fracturing proppant is a non-renewable resource, the nickel-iron slag has poor particle sphericity and compressive strength, cannot meet the use requirements of the oil fracturing proppant, and the nickel-iron slag has large discharge and is difficult to treat.
Description
Technical Field
The invention relates to the technical field of petroleum fracturing propping agents, in particular to a nickel-iron slag-based petroleum fracturing propping agent and a preparation method thereof.
Background
The ferronickel slag is water quenched slag of electric furnace, and has main components including silica, magnesia, iron oxide, etc. and is yellow, green and cyan. Has higher hardness, but poorer granularity and compressive strength, and can not meet the use requirements of the petroleum fracturing propping agent. The original form of the electric furnace water-quenched slag is irregular, if the electric furnace water-quenched slag is used as a base material to prepare the petroleum fracturing propping agent, the cost is high, and the sphericity of the product can be improved only through multi-section shaping, so that the using effect is achieved. Since the natural quartz sand for fracturing is used as the existing petroleum fracturing propping agent and is a non-renewable mineral resource, a new petroleum fracturing propping agent needs to be developed to replace the existing natural quartz sand for fracturing.
The process of smelting ferronickel alloy by a pyrogenic process and extracting nickel metal from laterite-nickel ore can generate a large amount of ferronickel slag, the ferronickel slag has the problems of large discharge amount and difficult treatment, the ferronickel slag is the fourth large smelting slag in China after iron slag, steel slag and red mud, the comprehensive utilization rate is less than 10%, and the large amount of ferronickel slag not only occupies land, but also has serious influence on the surrounding ecological environment. The content of nickel-iron slag exceeds50% SiO210% to 30% of Al2O3And 10 to 20 percent of MgO, wherein the MgO in the nickel-iron slag stably exists in the form of forsterite or spinel, the problem of volume expansion cannot occur, and the performance is stable.
Disclosure of Invention
The invention provides a ferronickel slag-based petroleum fracturing propping agent and a preparation method thereof, overcomes the defects of the prior art, and can effectively solve the problems that the natural quartz sand for fracturing of the conventional petroleum fracturing propping agent is a non-renewable resource, the ferronickel slag has poor particle sphericity and compressive strength, cannot meet the use requirement of the petroleum fracturing propping agent, and the ferronickel slag has large discharge and is difficult to treat.
One of the technical schemes of the invention is realized by the following measures: a nickel-iron slag-based petroleum fracturing propping agent is obtained by the following steps: step one, uniformly mixing required amounts of a binder, a diluent, a curing agent and powder to obtain a mixed material, wherein the weight ratio of the binder to the diluent to the curing agent to the powder is 2.5-8.0: 1: 1: 15; and secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain the nickel-iron slag-based petroleum fracturing propping agent, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1: 0.04-0.25.
The following is a further optimization or/and improvement of one of the above-mentioned technical solutions of the invention:
the binder is more than one of phenolic resin and epoxy resin.
The phenolic resin is thermosetting phenolic resin with viscosity of 10Pa.s to 10000mPa.s, and the epoxy resin is epoxy resin with epoxy value of 0.42 to 0.55.
The diluent is an epoxy reactive diluent.
The epoxy active diluent is one of epoxypropane butyl ether, epoxypropane benzyl ether, methacrylic acid-beta-hydroxyethyl and C12-14 alkyl glycidyl ether.
The curing agent is more than one of aromatic amine curing agent, acid anhydride curing agent, dicyandiamide curing agent and imidazole curing agent.
The aromatic amine curing agent is one of m-phenylenediamine, m-xylylenediamine, 4 '-diaminodiphenyl sulfone and 4, 4' -diaminodiphenyl methane, the anhydride curing agent is one of 2-ethyl-4-methylimidazole and maleic anhydride, the dicyandiamide curing agent is dicyandiamide, and the imidazole curing agent is one of imidazole, 2-methylimidazole and 2-ethylimidazole.
The powder is more than one of quartz powder and ferronickel slag powder with the granularity less than or equal to 106 mu m.
In the second step, the rotating speed is adjusted to 800r/min to 1000r/min during stirring, the stirring rotating speed is reduced to 400r/min to 600r/min when the temperature of the materials reaches 60 ℃ to 80 ℃, the stirring rotating speed is reduced to 200r/min to 400r/min when the temperature of the materials is 40 ℃ to 50 ℃, and the stirring time is 15min to 20 min.
In the second step, microparticles having a particle size of 850 to 425 μm are obtained after sieving.
In the second step, the primarily shaped ferronickel slag is the ferronickel slag which is crushed and screened to obtain the ferronickel slag with the granularity of 850 to 106 microns; the ferronickel slag after secondary shaping is obtained by stirring and screening the ferronickel slag after primary shaping at high speed, and the granularity of the ferronickel slag is 850-425 mu m.
The second technical scheme of the invention is realized by the following measures: a preparation method of a ferronickel slag-based petroleum fracturing propping agent comprises the following steps: step one, uniformly mixing required amounts of a binder, a diluent, a curing agent and powder to obtain a mixed material, wherein the weight ratio of the binder to the diluent to the curing agent to the powder is 2.5-8.0: 1: 1: 15; and secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain the nickel-iron slag-based petroleum fracturing propping agent, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1: 0.04-0.25.
The following is further optimization or/and improvement of the second technical scheme of the invention:
the binder is more than one of phenolic resin and epoxy resin.
The phenolic resin is thermosetting phenolic resin with viscosity of 10Pa.s to 10000mPa.s, and the epoxy resin is epoxy resin with epoxy value of 0.42 to 0.55.
The diluent is an epoxy reactive diluent.
The epoxy active diluent is one of epoxypropane butyl ether, epoxypropane benzyl ether, methacrylic acid-beta-hydroxyethyl and C12-14 alkyl glycidyl ether.
The curing agent is more than one of aromatic amine curing agent, acid anhydride curing agent, dicyandiamide curing agent and imidazole curing agent.
The aromatic amine curing agent is one of m-phenylenediamine, m-xylylenediamine, 4 '-diaminodiphenyl sulfone and 4, 4' -diaminodiphenyl methane, the anhydride curing agent is one of 2-ethyl-4-methylimidazole and maleic anhydride, the dicyandiamide curing agent is dicyandiamide, and the imidazole curing agent is one of imidazole, 2-methylimidazole and 2-ethylimidazole.
The powder is more than one of quartz powder and ferronickel slag powder with the granularity less than or equal to 106 mu m.
In the second step, the rotating speed is adjusted to 800r/min to 1000r/min during stirring, the stirring rotating speed is reduced to 400r/min to 600r/min when the temperature of the materials reaches 60 ℃ to 80 ℃, the stirring rotating speed is reduced to 200r/min to 400r/min when the temperature of the materials is 40 ℃ to 50 ℃, and the stirring time is 15min to 20 min.
In the second step, microparticles having a particle size of 850 to 425 μm are obtained after sieving.
In the second step, the primarily shaped ferronickel slag is the ferronickel slag which is crushed and screened to obtain the ferronickel slag with the granularity of 850 to 106 microns; the ferronickel slag after secondary shaping is obtained by stirring and screening the ferronickel slag after primary shaping at high speed, and the granularity of the ferronickel slag is 850-425 mu m.
The ferronickel slag-based petroleum fracturing propping agent is obtained by performing multi-stage shaping on ferronickel slag and then modifying the ferronickel slag and mixed materials, has good sphericity, low volume weight and good compressive strength, can meet the use requirement of the petroleum fracturing propping agent, simultaneously realizes resource utilization of solid wastes, and effectively solves the problems that the natural quartz sand for fracturing of the existing petroleum fracturing propping agent is a non-renewable resource, the ferronickel slag has poor particle sphericity and compressive strength, cannot meet the use requirement of the petroleum fracturing propping agent, and the ferronickel slag has large discharge and is difficult to treat.
Drawings
FIG. 1 is a figure of the nickel-iron slag of the present invention under the condition that the microscope magnification is 30 times.
FIG. 2 is a shape diagram of the ferronickel slag after primary shaping in the invention under the condition that the microscope magnification is 30 times.
FIG. 3 is a shape diagram of the ferronickel slag after the secondary shaping in the invention under the condition that the microscope magnification is 30 times.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. The various chemical reagents and chemical articles mentioned in the invention are all the chemical reagents and chemical articles which are well known and commonly used in the prior art, unless otherwise specified; the percentages in the invention are mass percentages unless otherwise specified; the solution in the present invention is an aqueous solution in which the solvent is water, for example, a hydrochloric acid solution is an aqueous hydrochloric acid solution, unless otherwise specified; the normal temperature and room temperature in the present invention generally mean a temperature of 15 ℃ to 25 ℃, and are generally defined as 25 ℃.
The invention is further described below with reference to the following examples:
example 1: the ferronickel slag-based petroleum fracturing propping agent is obtained by the following steps: step one, uniformly mixing required amounts of a binder, a diluent, a curing agent and powder to obtain a mixed material, wherein the weight ratio of the binder to the diluent to the curing agent to the powder is 2.5-8.0: 1: 1: 15; and secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain the nickel-iron slag-based petroleum fracturing propping agent, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1: 0.04-0.25.
After the ferronickel slag with clear edges is primarily shaped, the sphericity of ferronickel slag particles can be improved, the secondary shaping time can be shortened, the energy consumption is reduced, and the efficiency is improved; the ferronickel slag-based petroleum fracturing propping agent provided by the invention is characterized in that ferronickel slag is crushed and screened to obtain primary shaped ferronickel slag, the primary shaped ferronickel slag is stirred at a high speed and screened to obtain secondary shaped ferronickel slag, then the primary shaped ferronickel slag is bonded and coated on the surface of the primary shaped and secondary shaped ferronickel slag particles by using a binder, and a modified layer forms an inorganic and organic composite layer, so that the volume weight of the ferronickel slag is reduced, the strength of the ferronickel slag is improved, and meanwhile, the using requirement of the petroleum fracturing propping agent can be met, so that the ferronickel slag-based petroleum fracturing propping agent is good in sphericity, low in volume weight, not easy to expand and good in compressive strength.
Example 2: the ferronickel slag-based petroleum fracturing propping agent is obtained by the following steps: step one, uniformly mixing required amounts of a binder, a diluent, a curing agent and powder to obtain a mixed material, wherein the weight ratio of the binder to the diluent to the curing agent to the powder is 2.5 or 8.0: 1: 1: 15; and secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain the nickel-iron slag-based petroleum fracturing propping agent, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1:0.04 or 0.25.
Example 3: in the optimization of the embodiment, the binder is more than one of phenolic resin and epoxy resin.
Example 4: as optimization of the above embodiment, the phenol resin is a thermosetting phenol resin having a viscosity of 10pa.s to 10000mpa.s, and the epoxy resin is an epoxy resin having an epoxy value of 0.42 to 0.55.
Example 5: as an optimization of the above example, the diluent is an epoxy reactive diluent.
Example 6: as optimization of the above embodiment, the epoxy reactive diluent is one of propylene oxide butyl ether, propylene oxide benzyl ether, beta-hydroxyethyl methacrylate and C12-14 alkyl glycidyl ether.
Example 7: in the optimization of the above embodiment, the curing agent is one or more of aromatic amine curing agent, acid anhydride curing agent, dicyandiamide curing agent and imidazole curing agent.
Example 8: as an optimization of the above embodiment, the aromatic amine curing agent is one of m-phenylenediamine, m-xylylenediamine, 4 '-diaminodiphenyl sulfone, and 4, 4' -diaminodiphenyl methane, the acid anhydride curing agent is one of 2-ethyl-4-methylimidazole and maleic anhydride, the dicyandiamide curing agent is dicyandiamide, and the imidazole curing agent is one of imidazole, 2-methylimidazole, and 2-ethylimidazole.
Example 9: as the optimization of the embodiment, the powder is more than one of quartz powder and ferronickel slag powder with the granularity less than or equal to 106 mu m.
In the invention, the powder can adopt quartz powder with the granularity of less than or equal to 106 mu m, ferronickel slag powder with the granularity of less than or equal to 106 mu m and mixed powder of the quartz powder with the granularity of less than or equal to 106 mu m and the ferronickel slag powder, and the weight ratio of the quartz powder with the granularity of less than or equal to 106 mu m to the ferronickel slag powder is 7: 3, and mixing.
Example 10: as the optimization of the embodiment, in the second step, the rotating speed during stirring is adjusted to 800r/min to 1000r/min, when the material temperature reaches 60 ℃ to 80 ℃, the stirring rotating speed is reduced to 400r/min to 600r/min, when the material temperature is 40 ℃ to 50 ℃, the stirring rotating speed is reduced to 200r/min to 400r/min, and the stirring time is 15min to 20 min.
Example 11: as an optimization of the above example, in the second step, the sieving gives microparticles with a size of 850 μm to 425 μm.
Example 12: as the optimization of the above embodiment, in the second step, the primarily shaped ferronickel slag is the ferronickel slag, which is crushed and sieved to obtain the ferronickel slag with the particle size of 850 μm to 106 μm; the ferronickel slag after secondary shaping is obtained by stirring and screening the ferronickel slag after primary shaping at high speed, and the granularity of the ferronickel slag is 850-425 mu m.
In the invention, the ferronickel slag is crushed and sieved to obtain primary shaped ferronickel slag with the granularity of more than 850 mu m, the granularity of 850-106 mu m and the granularity of less than 106 mu m, and the ferronickel slag with the granularity of 850-106 mu m is stirred at high speed and sieved to obtain the ferronickel slag with the granularity of 850-425 mu m, 600-300 mu m, 425-212 mu m and 212-106 mu m.
Example 13: the ferronickel slag-based petroleum fracturing propping agent is obtained by the following steps: step one, uniformly mixing required amounts of phenolic resin, epoxy active diluent, aromatic amine curing agent and quartz powder (the granularity is less than or equal to 106 microns) to obtain a mixed material, wherein the weight ratio of the phenolic resin to the epoxy active diluent to the aromatic amine curing agent to the quartz powder (the granularity is less than or equal to 106 microns) is 2.5: 1: 1: 15; secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain a nickel-iron slag-based petroleum fracturing propping agent with the granularity of 850-425 microns, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1:0.04, and the nickel-iron slag subjected to primary shaping is crushed and screened to obtain nickel-iron slag with the granularity of 850-106 microns; the ferronickel slag after secondary shaping is obtained by stirring and screening the ferronickel slag after primary shaping at high speed, wherein the granularity of the ferronickel slag is 850-425 μm; the rotating speed is adjusted to 800r/min during stirring, the stirring rotating speed is reduced to 400r/min when the material temperature reaches 60 ℃, and the stirring rotating speed is reduced to 200r/min when the material temperature reaches 40 ℃, and the stirring time is 15 min.
Example 14: the ferronickel slag-based petroleum fracturing propping agent is obtained by the following steps: step one, uniformly mixing required amount of epoxy resin, epoxy active diluent, anhydride curing agent and ferronickel slag powder (the granularity is less than or equal to 106 mu m) to obtain a mixed material, wherein the weight ratio of the epoxy resin, the epoxy active diluent, the anhydride curing agent and the ferronickel slag powder (the granularity is less than or equal to 106 mu m) is 8.0: 1: 1: 15; secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain a nickel-iron slag-based petroleum fracturing propping agent with the granularity of 850-425 microns, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1:0.25, and the nickel-iron slag subjected to primary shaping is crushed and screened to obtain nickel-iron slag with the granularity of 850-106 microns; the ferronickel slag after secondary shaping is obtained by stirring and screening the ferronickel slag after primary shaping at high speed, wherein the granularity of the ferronickel slag is 850-425 μm; the rotation speed is adjusted to 1000r/min during stirring, when the material temperature reaches 80 ℃, the stirring rotation speed is reduced to 600r/min, when the material temperature is 50 ℃, the stirring rotation speed is reduced to 400r/min, and the stirring time is 20 min.
Example 15: the ferronickel slag-based petroleum fracturing propping agent is obtained by the following steps: the first step, uniformly mixing required amount of epoxy resin, epoxy active diluent, dicyandiamide curing agent and mixed powder (mixed powder with the weight ratio of quartz powder with the granularity of less than or equal to 106 mu m to ferronickel slag powder of 7: 3) to obtain a mixed material, wherein the weight ratio of the epoxy resin, the epoxy active diluent, the dicyandiamide curing agent to the mixed powder (mixed powder with the weight ratio of quartz powder with the granularity of less than or equal to 106 mu m to ferronickel slag powder of 7: 3) is 4.0: 1: 1: 15; secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain a nickel-iron slag-based petroleum fracturing propping agent with the granularity of 850-425 microns, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1:0.10, and the nickel-iron slag subjected to primary shaping is crushed and screened to obtain nickel-iron slag with the granularity of 850-106 microns; the rotating speed is adjusted to 900r/min during stirring, when the material temperature reaches 70 ℃, the stirring rotating speed is reduced to 500r/min, when the material temperature is 45 ℃, the stirring rotating speed is reduced to 300r/min, and the stirring time is 18 min.
Example 16: firstly, putting 1000kg of dried ferronickel slag into an impact crusher, obtaining ferronickel slag with the granularity of more than 850 mu m, 850-106 mu m and less than 106 mu m after primary shaping of crushing and screening, returning the ferronickel slag with the granularity of more than 850 mu m into the impact crusher, taking the ferronickel slag with the granularity of less than 106 mu m as powder for standby, putting the ferronickel slag with the granularity of 850-106 mu m into a high-speed stirrer, and obtaining the ferronickel slag with the granularity of 850-425 mu m after secondary shaping of high-speed stirring and screening; then, uniformly mixing 320g of epoxy resin, 40g of epoxypropane benzyl ether, 40g of 4, 4' -diaminodiphenylmethane and 600g of quartz powder (the granularity is less than or equal to 106 mu m) to obtain a mixed material, finally, placing 2000g of ferronickel slag with the granularity of 850 mu m to 425 mu m and 100g of the mixed material in a high-speed stirrer, mixing and stirring under the condition that the stirring speed is 800r/min, reducing the stirring speed to 400r/min when the temperature of the high-speed stirrer reaches 60 ℃, reducing the stirring speed to 200r/min when the temperature of the high-speed stirrer is 40 ℃, stirring for 15min, and screening to obtain the ferronickel slag-based petroleum fracturing propping agent with the granularity of 850 mu m to 425 mu m.
Example 17: firstly, putting 1000kg of dried ferronickel slag into an impact crusher, obtaining ferronickel slag with the granularity of more than 850 mu m, 850-106 mu m and less than 106 mu m after primary shaping of crushing and screening, returning the ferronickel slag with the granularity of more than 850 mu m into the impact crusher, taking the ferronickel slag with the granularity of less than 106 mu m as powder for standby, putting the ferronickel slag with the granularity of 850-106 mu m into a high-speed stirrer, and obtaining the ferronickel slag with the granularity of 850-425 mu m after secondary shaping of high-speed stirring and screening; then, uniformly mixing 320g of epoxy resin, 40g of epoxypropane benzyl ether, 40g of 4, 4' -diaminodiphenylmethane and 600g of ferronickel slag powder (the particle size is less than or equal to 106 mu m) to obtain a mixed material, finally, placing 2000g of ferronickel slag with the particle size of 850 mu m to 425 mu m and 100g of the mixed material in a high-speed stirrer, mixing and stirring under the condition that the stirring speed is 800r/min, reducing the stirring speed to 400r/min when the temperature of the high-speed stirrer reaches 60 ℃, reducing the stirring speed to 200r/min when the temperature of the high-speed stirrer is 40 ℃, stirring for 15min, and screening to obtain the ferronickel slag-based petroleum fracturing propping agent with the particle size of 850 mu m to 425 mu m.
Example 18: firstly, putting 1000kg of dried ferronickel slag into an impact crusher, obtaining ferronickel slag with the granularity of more than 850 mu m, 850-106 mu m and less than 106 mu m after primary shaping of crushing and screening, returning the ferronickel slag with the granularity of more than 850 mu m into the impact crusher, taking the ferronickel slag with the granularity of less than 106 mu m as powder for standby, putting the ferronickel slag with the granularity of 850-106 mu m into a high-speed stirrer, and obtaining the ferronickel slag with the granularity of 850-425 mu m after secondary shaping of high-speed stirring and screening; then, uniformly mixing 100g of epoxy resin, 40g of C12-14 alkyl glycidyl ether, 40g of 4, 4' -diaminodiphenylmethane and 600g of quartz powder (the granularity is less than or equal to 106 mu m) to obtain a mixed material, finally, placing 2000g of ferronickel slag with the granularity of 850 mu m to 425 mu m and 100g of the mixed material in a high-speed stirrer, mixing and stirring under the condition that the stirring speed is 1000r/min, reducing the stirring speed to 600r/min when the temperature of the high-speed stirrer reaches 80 ℃, reducing the stirring speed to 400r/min when the temperature of the high-speed stirrer is 50 ℃, stirring for 20min, and screening to obtain the ferronickel slag-based petroleum fracturing propping agent with the granularity of 850 mu m to 425 mu m.
Example 19: firstly, putting 1000kg of dried ferronickel slag into an impact crusher, obtaining ferronickel slag with the granularity of more than 850 mu m, 850-106 mu m and less than 106 mu m after primary shaping of crushing and screening, returning the ferronickel slag with the granularity of more than 850 mu m into the impact crusher, taking the ferronickel slag with the granularity of less than 106 mu m as powder for standby, putting the ferronickel slag with the granularity of 850-106 mu m into a high-speed stirrer, and obtaining the ferronickel slag with the granularity of 850-425 mu m after secondary shaping of high-speed stirring and screening; then, uniformly mixing 100g of epoxy resin, 40g of C12-14 alkyl glycidyl ether, 40g of 4, 4' -diaminodiphenylmethane and 600g of mixed powder (formed by mixing quartz powder with the granularity of less than or equal to 106 mu m and ferronickel slag powder in a weight ratio of 7: 3) to obtain a mixed material, finally placing 2000g of ferronickel slag with the granularity of 850 mu m to 425 mu m and 100g of the mixed material in a high-speed stirrer, mixing and stirring at the stirring speed of 1000r/min, reducing the stirring speed to 600r/min when the temperature of the high-speed stirrer reaches 80 ℃, reducing the stirring speed to 400r/min when the temperature of the high-speed stirrer is 50 ℃, stirring for 20min, and screening to obtain the ferronickel slag-based petroleum fracturing propping agent with the granularity of 850 mu m to 425 mu m.
Example 20: firstly, putting 1000kg of dried ferronickel slag into an impact crusher, obtaining ferronickel slag with the granularity of more than 850 mu m, 850-106 mu m and less than 106 mu m after primary shaping of crushing and screening, returning the ferronickel slag with the granularity of more than 850 mu m into the impact crusher, taking the ferronickel slag with the granularity of less than 106 mu m as powder for standby, putting the ferronickel slag with the granularity of 850-106 mu m into a high-speed stirrer, and obtaining the ferronickel slag with the granularity of 850-425 mu m after secondary shaping of high-speed stirring and screening; then, 100g of epoxy resin, 40g of C12-14 alkyl glycidyl ether, 40g of 4, 4' -diaminodiphenylmethane and 600g of quartz powder (the granularity is less than or equal to 106 mu m) are uniformly mixed to obtain a mixed material, finally, 2000g of nickel-iron slag with the granularity of 850 mu m to 425 mu m and 500g of the mixed material are placed in a high-speed stirrer, the mixed material is stirred at the stirring speed of 900r/min, when the temperature of the high-speed stirrer reaches 70 ℃, the stirring speed is reduced to 500r/min, when the temperature of the high-speed stirrer is 45 ℃, the stirring speed is reduced to 300r/min, and after stirring for 18min, the nickel-iron slag-based petroleum fracturing propping agent with the granularity of 850 mu m to 425 mu m is obtained by screening.
The following are the investigation of the performance of the ferronickel slag-based petroleum fracturing propping agent of the invention:
the test method comprises the following steps: the ferronickel slag-based petroleum fracturing propping agent obtained in the embodiments 16 to 20 of the invention is subjected to performance test, meanwhile, the existing petroleum fracturing propping agent is used as a comparative example, the existing petroleum fracturing propping agent is natural quartz sand for fracturing, and the sphericity, volume weight (volume density) and breakage rate are tested according to SY/T5108-2014 proppant performance test method for hydraulic fracturing and gravel filling operations.
And (3) test results: as shown in table 1, the ferronickel slag-based petroleum fracturing propping agent obtained in examples 16 to 20 of the invention has good sphericity; as shown in fig. 1 to 3, after the nickel-iron slag is shaped in multiple stages, the sphericity of the nickel-iron slag becomes better and better; compared with the nickel-iron slag, the nickel-iron slag-based petroleum fracturing propping agent obtained in the embodiments 16 to 20 of the invention has low volume weight (volume density); compared with the existing petroleum fracturing propping agent and the ferronickel slag, the ferronickel slag-based petroleum fracturing propping agent obtained in the embodiments 16 to 20 of the invention has low breaking rate under the closed pressure condition of 52MPa, and the result shows that the ferronickel slag-based petroleum fracturing propping agent has good sphericity, low volume weight (volume density) and difficult expansion and good compressive strength.
In conclusion, the ferronickel slag-based petroleum fracturing propping agent is obtained by performing multi-stage shaping on the ferronickel slag and then modifying the ferronickel slag and a mixed material, has good sphericity, low volume weight and good compressive strength, can meet the use requirement of the petroleum fracturing propping agent, realizes resource utilization of solid waste, and effectively solves the problems that the natural quartz sand for fracturing of the existing petroleum fracturing propping agent is a non-renewable resource, the ferronickel slag has poor particle sphericity and compressive strength, cannot meet the use requirement of the petroleum fracturing propping agent, and the ferronickel slag has large discharge and is difficult to treat.
The technical characteristics form an embodiment of the invention, which has strong adaptability and implementation effect, and unnecessary technical characteristics can be increased or decreased according to actual needs to meet the requirements of different situations.
Claims (10)
1. A ferronickel slag-based petroleum fracturing propping agent is characterized by being prepared by the following steps: step one, uniformly mixing required amounts of a binder, a diluent, a curing agent and powder to obtain a mixed material, wherein the weight ratio of the binder to the diluent to the curing agent to the powder is 2.5-8.0: 1: 1: 15; and secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain the nickel-iron slag-based petroleum fracturing propping agent, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1: 0.04-0.25.
2. The ferronickel slag-based petroleum fracturing proppant as set forth in claim 1, characterized in that the binder is one or more of phenolic resin and epoxy resin; or/and the diluent is an epoxy reactive diluent.
3. The ferronickel slag-based petroleum fracturing propping agent of claim 2, characterized in that the phenolic resin is a thermosetting phenolic resin with a viscosity of 10pa.s to 10000mpa.s, and the epoxy resin is an epoxy resin with an epoxy value of 0.42 to 0.55; or/and the epoxy reactive diluent is one of propylene oxide butyl ether, propylene oxide benzyl ether, methacrylic acid-beta-hydroxyethyl ester and C12-14 alkyl glycidyl ether.
4. The ferronickel slag-based petroleum fracturing propping agent according to claim 1, 2 or 3, characterized in that the curing agent is one or more of aromatic amine curing agent, acid anhydride curing agent, dicyandiamide curing agent and imidazole curing agent.
5. The ferronickel slag-based petroleum fracturing propping agent of claim 4, characterized in that the aromatic amine curing agent is one of m-phenylenediamine, m-xylylenediamine, 4 '-diaminodiphenyl sulfone and 4, 4' -diaminodiphenyl methane; or/and the acid anhydride curing agent is one of 2-ethyl-4-methylimidazole and maleic anhydride, and the dicyandiamide curing agent is dicyandiamide; or/and the imidazole curing agent is one of imidazole, 2-methylimidazole and 2-ethylimidazole.
6. The ferronickel slag-based petroleum fracturing propping agent as claimed in claim 1, 2, 3 or 5, characterized in that the powder is one or more of quartz powder and ferronickel slag powder with a particle size of 106 μm or less; or/and in the second step, the rotating speed is adjusted to 800r/min to 1000r/min during stirring, the stirring rotating speed is reduced to 400r/min to 600r/min when the temperature of the materials reaches 60 ℃ to 80 ℃, the stirring rotating speed is reduced to 200r/min to 400r/min when the temperature of the materials is 40 ℃ to 50 ℃, and the stirring time is 15min to 20 min.
7. The ferronickel slag-based petroleum fracturing propping agent according to claim 4, characterized in that the powder is more than one of quartz powder and ferronickel slag powder with the particle size of less than or equal to 106 μm; or/and in the second step, the rotating speed is adjusted to 800r/min to 1000r/min during stirring, the stirring rotating speed is reduced to 400r/min to 600r/min when the temperature of the materials reaches 60 ℃ to 80 ℃, the stirring rotating speed is reduced to 200r/min to 400r/min when the temperature of the materials is 40 ℃ to 50 ℃, and the stirring time is 15min to 20 min.
8. The ferronickel slag-based petroleum fracturing proppant of claim 1, 2, 3, 5 or 7, characterized in that in the second step, micron particles with a particle size of 850 to 425 μm are obtained after sieving; or/and in the second step, the primarily shaped ferronickel slag is the ferronickel slag which is crushed and screened to obtain the ferronickel slag with the granularity of 850 to 106 mu m; the ferronickel slag after secondary shaping is obtained by stirring and screening the ferronickel slag after primary shaping at high speed, and the granularity of the ferronickel slag is 850-425 mu m.
9. The ferronickel slag-based petroleum fracturing propping agent according to claim 4 or 6, characterized in that in the second step, micron particles with the particle size of 850-425 μm are obtained after sieving; or/and in the second step, the primarily shaped ferronickel slag is the ferronickel slag which is crushed and screened to obtain the ferronickel slag with the granularity of 850 to 106 mu m; the ferronickel slag after secondary shaping is obtained by stirring and screening the ferronickel slag after primary shaping at high speed, and the granularity of the ferronickel slag is 850-425 mu m.
10. A method for preparing a ferronickel slag-based petroleum fracturing proppant according to any one of claims 2 to 9, characterized by comprising the following steps: step one, uniformly mixing required amounts of a binder, a diluent, a curing agent and powder to obtain a mixed material, wherein the weight ratio of the binder to the diluent to the curing agent to the powder is 2.5-8.0: 1: 1: 15; and secondly, adding a required amount of mixed materials into the nickel-iron slag subjected to primary shaping and secondary shaping, mixing and stirring, and screening to obtain the nickel-iron slag-based petroleum fracturing propping agent, wherein the weight ratio of the nickel-iron slag to the mixed materials is 1: 0.04-0.25.
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