CN114349475B - Preparation method of core-shell type ceramsite fracturing propping agent for oil and gas collection - Google Patents

Preparation method of core-shell type ceramsite fracturing propping agent for oil and gas collection Download PDF

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CN114349475B
CN114349475B CN202210274269.3A CN202210274269A CN114349475B CN 114349475 B CN114349475 B CN 114349475B CN 202210274269 A CN202210274269 A CN 202210274269A CN 114349475 B CN114349475 B CN 114349475B
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propping agent
core
fracturing propping
drying
slurry
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CN114349475A (en
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马超
张华辉
王鹏
徐龙
袁在涛
王清
于波
黄宗魁
张晓蕾
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Shengli Oilfield Fangyuan Ceramics Co ltd
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/132Waste materials; Refuse; Residues
    • C04B33/1321Waste slurries, e.g. harbour sludge, industrial muds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/80Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
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Abstract

The invention relates to a preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection, which comprises the following steps: (1) and grinding the municipal sludge containing the organic matters into powder, and then granulating and drying to obtain the kernel precursor. (2) And uniformly mixing clay and waste iron powder, and then adding water and uniformly stirring to obtain the inner cladding layer slurry. (3) And mixing clay and water, and uniformly stirring to obtain the outer coating layer slurry. (4) And immersing the core precursor into the slurry of the inner coating layer to uniformly coat the outer surface of the core precursor, taking out the core precursor for drying, immersing the obtained particles into the slurry of the outer coating layer again to uniformly coat the outer surface of the particles, taking out the particles for drying, uniformly placing the particles after the drying, calcining, and obtaining the ceramsite fracturing propping agent after the calcining. The core-shell fracturing propping agent disclosed by the invention is low in density and good in compressive property, and the purpose of reducing the density of the fracturing propping agent and keeping the good compressive property of the fracturing propping agent is realized.

Description

Preparation method of core-shell type ceramsite fracturing propping agent for oil and gas collection
Technical Field
The invention relates to the technical field of fracturing propping agents, in particular to a preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection.
Background
The fracturing propping agent is mainly used for fracturing reformation of a deep well and a high-pressure oil-gas layer, and is injected into a fractured rock stratum crack through high-pressure carrier fluid to play a role in supporting the crack to be not closed due to stress release, so that high flow conductivity is kept, oil gas is smooth, and the yield is increased. Practice proves that the fracturing after the fracturing propping agent is added can improve the yield by more than 30 percent, and effectively improves the oil gas collection efficiency.
The main raw material of the traditional fracturing propping agent is bauxite, the bauxite is crushed and finely ground into micro powder, the micro powder is compounded with an additive, and then the sintering is carried out at high temperature, the main crystal phase after the sintering is usually corundum phase, the density of the corundum phase is higher, the density of the propping agent is higher, and the subsequent carrying of the propping agent into a rock stratum by using a carrier fluid is influenced. But the density of the fracturing propping agent is not too low, otherwise, the compressive strength of the fracturing propping agent can not meet the requirement easily.
In order to overcome the problems, some researches have achieved certain results by using composite raw materials to prepare low-density fracturing propping agents, but the technologies generally have the problems of complex process, high cost of the adopted raw materials, unsuitability for large-scale production and the like, and more importantly, the density of the fracturing propping agent is not well reduced, and meanwhile, the good pressure resistance of the fracturing propping agent is not maintained, so that the comprehensive performance of the fracturing propping agent is poor.
Disclosure of Invention
Aiming at the problems, the invention provides the ceramsite fracturing propping agent for oil and gas collection and the preparation method thereof.
In order to achieve the purpose, the invention discloses the following technical scheme:
a preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) and grinding the municipal sludge containing the organic matters into powder, and then granulating and drying to obtain the kernel precursor.
(2) And uniformly mixing clay and waste iron powder, and then adding water and uniformly stirring to obtain the inner cladding layer slurry.
(3) And mixing clay and water, and uniformly stirring to obtain the outer coating layer slurry.
(4) And immersing the core precursor into the slurry of the inner coating layer to uniformly coat the outer surface of the core precursor, taking out the core precursor for drying, immersing the obtained particles into the slurry of the outer coating layer again to uniformly coat the outer surface of the particles, taking out the particles for drying, uniformly placing the particles after the drying, calcining, and obtaining the ceramsite fracturing propping agent after the calcining.
Further, in the step (1), the water content of the granulated sludge particles is controlled to be 35-40%.
Further, in the step (1), the drying temperature is 120-150 ℃, the drying time is 1.5-3 hours, and organic matter components in municipal sludge particles can be removed by drying at a high temperature for a long time, so that the obtained inner core precursor has a low-density porous structure.
Further, in the step (1), the diameter of the core precursor is controlled to be 0.5-0.8 mm.
Further, in the step (2), the proportion of the clay to the waste iron powder is 1 part by weight: 0.3 to 0.5 part by weight. After the inner cladding layer containing high-content iron powder is sintered at high temperature, an iron-based ceramic inner cladding layer can be formed, and good pressure resistance is provided for the fracturing propping agent.
Further, in the step (2), the solid content of the inner coating layer slurry is kept between 18 and 22 percent, so that the slurry can be coated on the surface of the inner core precursor better.
Further, in the step (3), the solid content of the outer coating layer slurry is kept between 15% and 20%, so that the slurry can be better coated on the surface of the inner coating layer on the surface of the inner core precursor.
Further, in the step (4), the drying temperature is 80-90 ℃, and the drying time is 50-80 min.
Further, in the step (4), the calcining temperature is 1350-1420 ℃, the calcining time is 1-2 hours, the ceramsite fracturing propping agent is formed by calcining the core precursor, the inner cladding layer and the outer cladding layer at a high temperature, and meanwhile, the inner cladding layer is ferrated at a high temperature, so that the inner cladding layer has good pressure resistance.
Further, in the step (4), the thickness of the inner cladding layer of the ceramsite fracturing propping agent is 0.3-0.5 mm, and the thickness of the outer cladding layer is 0.1-0.2 mm.
Compared with the prior art, the invention has the following beneficial effects: the core-shell fracturing propping agent disclosed by the invention is low in density and good in compressive property, and the purpose of reducing the density of the fracturing propping agent and simultaneously keeping the good compressive property of the fracturing propping agent is realized, and the main reasons are as follows:
the method utilizes the characteristic that the municipal sludge contains a large amount of organic matter components as the inner core of the fracturing propping agent, and the organic matter components in the inner core are fully volatilized and combusted after subsequent high-temperature long-time heating, so that the inner core is of a porous structure, and the integral density of the fracturing propping agent can be effectively reduced. Meanwhile, the method has the technical advantages of low cost, easily obtained raw materials and realization of resource utilization of the municipal sludge by taking the municipal sludge as the raw material.
Further, the clay and the waste iron powder are used as raw materials, the inner cladding layer with high iron powder content is prepared on the surface of the inner core, and the inner cladding layer is calcined at high temperature to form an iron-based ceramic inner cladding layer, so that the excellent compression resistance can be provided for the fracturing propping agent.
Furthermore, the surface of the inner coating layer is also coated with an outer coating layer, and the outer coating layer is subjected to high-temperature calcination to form a ceramic outer coating layer, so that the fracturing propping agent has good compression resistance, can play a role in protecting the inner coating layer from being corroded, prolongs the service life of the fracturing propping agent, and meanwhile, the components of the outer coating layer and the inner coating layer have good continuity, so that the bonding force between the components and the inner coating layer can be increased, and the falling of the outer coating layer is reduced.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. The invention will now be further illustrated by specific examples.
In the following examples, the municipal sludge is a sewage treatment plant from a city. The sludge is detected to contain 43.8 percent of organic matters by mass fraction.
Example 1
A preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) drying the municipal sludge, grinding the dried municipal sludge into powder, then sieving the powder by a 400-mesh sieve, placing the obtained sludge powder into a granulator for granulation, and simultaneously spraying atomized water vapor to form spherical particles with the average water content of 36%; the granules were dried at 140 ℃ for 2 hours to prepare a core precursor having an average diameter of about 0.6mm, for use.
(2) Respectively sieving clay powder and waste iron powder by a 400-mesh sieve, and then sieving the clay powder and the waste iron powder obtained by sieving according to 1 part by weight: 0.35 parts by weight of the components are mixed and then mechanically stirred for 30min to uniformly mix the components, and then clear water is added into the obtained mixed powder and continuously stirred to obtain inner coating layer slurry with the solid content of 18% for later use.
(3) And adding clear water into the clay powder obtained by sieving with a 400-mesh sieve, and continuously stirring to obtain outer coating layer slurry with the solid content of 16% for later use.
(4) And (3) immersing the core precursor into the coating layer slurry in the inner step (2) to uniformly coat the outer surface of the core precursor, taking out the core precursor, drying for 60min at 90 ℃, immersing the obtained particles into the outer coating layer slurry in the step (3) again to uniformly coat the outer surface of the particles, taking out the particles, drying for 50min at 80 ℃, putting the particles uniformly after the drying, calcining for 2 h at 1400 ℃, and cooling to room temperature along with a furnace after the drying to obtain the core-shell type ceramsite fracturing propping agent with the average thickness of the inner coating layer of 0.43mm and the average thickness of the outer coating layer of 0.2 mm.
Example 2
A preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) drying the municipal sludge, grinding the dried municipal sludge into powder, then sieving the powder by a 400-mesh sieve, placing the obtained sludge powder into a granulator for granulation, and simultaneously spraying atomized water vapor to form spherical particles with the average water content of 39%; the granules were dried at 150 ℃ for 1.5 hours to prepare a core precursor having an average diameter of about 0.8mm, for use.
(2) Respectively sieving clay powder and waste iron powder by a 400-mesh sieve, and then sieving the clay powder and the waste iron powder obtained by sieving according to 1 part by weight: 0.3 part by weight of the components are mixed and then mechanically stirred for 30min to uniformly mix the components, and then clear water is added into the obtained mixed powder and continuously stirred to obtain the inner coating layer slurry with the solid content of 22% for later use.
(3) And adding clear water into the clay powder obtained by sieving with a 400-mesh sieve, and continuously stirring to obtain outer coating layer slurry with the solid content of 20% for later use.
(4) And (3) immersing the core precursor into the coating layer slurry in the inner step (2) to enable the outer surface of the core precursor to be uniformly coated with slurry, taking out the core precursor to be dried at 90 ℃ for 70min, immersing the obtained particles into the outer coating layer slurry in the step (3) again to enable the outer surface of the particles to be uniformly coated with slurry, taking out the particles to be dried at 80 ℃ for 60min, putting the particles uniformly after the drying is finished, calcining the particles at 1350 ℃ for 2 hours, and cooling the particles to room temperature along with a furnace after the drying is finished to obtain the core-shell type ceramsite fracturing propping agent with the average thickness of the inner coating layer of 0.32mm and the average thickness of the outer coating layer of 0.18 mm.
Example 3
A preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) drying and grinding the municipal sludge, then sieving the powder by a 400-mesh sieve, placing the obtained sludge powder in a granulator for granulation, and simultaneously spraying atomized water vapor to enable the sludge powder to form spherical particles with the average water content of 35%; the granules were dried at 120 ℃ for 3 hours to prepare a core precursor having an average diameter of about 0.5mm, for use.
(2) Respectively sieving clay powder and waste iron powder by a 400-mesh sieve, and then sieving the clay powder and the waste iron powder obtained by sieving according to 1 part by weight: 0.45 part by weight of the components are mixed and then mechanically stirred for 30min to uniformly mix the components, and then clear water is added into the obtained mixed powder and continuously stirred to obtain the inner coating layer slurry with the solid content of 20% for later use.
(3) And adding clear water into the clay powder obtained by sieving with a 400-mesh sieve, and continuously stirring to obtain outer coating layer slurry with the solid content of 15% for later use.
(4) And (3) immersing the core precursor into the coating layer slurry in the inner step (2) to enable the outer surface of the core precursor to be uniformly coated with slurry, taking out the core precursor to be dried for 80min at 80 ℃, immersing the obtained particles into the outer coating layer slurry in the step (3) again to enable the outer surface of the particles to be uniformly coated with slurry, taking out the particles to be dried for 60min at 80 ℃, uniformly placing the particles after the drying, calcining for 1 h at 1400 ℃, and cooling to room temperature along with a furnace after the drying to obtain the core-shell type ceramsite fracturing propping agent with the average thickness of the inner coating layer of 0.3mm and the average thickness of the outer coating layer of 0.12 mm.
Example 4
A preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) drying the municipal sludge, grinding the dried municipal sludge into powder, then sieving the powder by a 400-mesh sieve, placing the obtained sludge powder into a granulator for granulation, and simultaneously spraying atomized water vapor to form spherical particles with the average water content of 40%; the granules were dried at 135 ℃ for 2.5 hours to prepare a core precursor having an average diameter of about 0.7mm, for use.
(2) Respectively sieving clay powder and waste iron powder by a 400-mesh sieve, and then sieving the clay powder and the waste iron powder obtained by sieving according to 1 part by weight: 0.5 parts by weight of the components are mixed and then mechanically stirred for 30min to uniformly mix the components, and then clear water is added into the obtained mixed powder and continuously stirred to obtain the inner coating layer slurry with the solid content of 21% for later use.
(3) And adding clear water into the clay powder obtained by sieving with a 400-mesh sieve, and continuously stirring to obtain outer coating layer slurry with the solid content of 18% for later use.
(4) And (3) immersing the core precursor into the coating layer slurry in the inner step (2) to uniformly coat the outer surface of the core precursor, taking out the core precursor, drying for 60min at 85 ℃, immersing the obtained particles into the outer coating layer slurry in the step (3) again to uniformly coat the outer surface of the particles, taking out the particles, drying for 60min at 80 ℃, putting the particles uniformly after the drying, calcining for 2 h at 1420 ℃, and cooling to room temperature along with a furnace after the drying to obtain the core-shell type ceramsite fracturing propping agent with the average thickness of the inner coating layer of 0.5mm and the average thickness of the outer coating layer of 0.2 mm.
Example 5
The preparation method of the core-shell type ceramsite fracturing propping agent for oil and gas collection is the same as that in example 1, and is characterized by comprising the following steps of (1): drying bauxite, grinding the bauxite into powder, sieving the powder by a 400-mesh sieve, placing the obtained sludge powder into a granulator for granulation, and simultaneously spraying atomized water vapor to enable the sludge powder to form spherical particles, wherein the average water content of the particles is 36%; the granules were dried at 140 ℃ for 2 hours to prepare a core precursor having an average diameter of about 0.6mm, for use.
Example 6
A preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) drying the municipal sludge, grinding the dried municipal sludge into powder, then sieving the powder by a 400-mesh sieve, placing the obtained sludge powder into a granulator for granulation, and simultaneously spraying atomized water vapor to form spherical particles with the average water content of 36%; the granules were dried at 140 ℃ for 2 hours to prepare a core precursor having an average diameter of about 0.6mm, for use.
(2) Respectively sieving clay powder and waste iron powder with a 400-mesh sieve, adding clear water into the clay powder obtained by sieving, and continuously stirring to obtain inner coating layer slurry with the solid content of 18% for later use.
(3) And adding clear water into the clay powder obtained by sieving with a 400-mesh sieve, and continuously stirring to obtain outer coating layer slurry with the solid content of 16% for later use.
(4) And (3) immersing the core precursor into the coating layer slurry in the inner step (2) to enable the outer surface of the core precursor to be uniformly coated with slurry, taking out the core precursor, drying for 60min at 90 ℃, immersing the obtained particles into the outer coating layer slurry in the step (3) again to enable the outer surface of the particles to be uniformly coated with slurry, taking out the particles, drying for 50min at 80 ℃, putting the particles uniformly after the drying, calcining for 2 hours at 1400 ℃, and cooling to room temperature along with a furnace after the drying is finished to obtain the core-shell type ceramsite fracturing propping agent.
Example 7
A preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) drying the municipal sludge, grinding the dried municipal sludge into powder, then sieving the powder by a 400-mesh sieve, placing the obtained sludge powder into a granulator for granulation, and simultaneously spraying atomized water vapor to form spherical particles with the average water content of 36%; the granules were dried at 140 ℃ for 2 hours to prepare a core precursor having an average diameter of about 0.6mm, for use.
(2) Respectively sieving clay powder and waste iron powder by a 400-mesh sieve, and then sieving the clay powder and the waste iron powder obtained by sieving according to 1 part by weight: 0.35 parts by weight of the components are mixed and then mechanically stirred for 30min to uniformly mix the components, and then clear water is added into the obtained mixed powder and continuously stirred to obtain inner coating layer slurry with the solid content of 18% for later use.
(3) And (3) immersing the core precursor into the coating layer slurry obtained in the inner step (2) to uniformly coat the outer surface of the core precursor, taking out the core precursor, drying for 60min at 90 ℃, uniformly placing the obtained particles after the drying, calcining for 2 h at 1400 ℃, and cooling to room temperature along with the furnace to obtain the core-shell type ceramsite fracturing propping agent.
Example 8
A preparation method of a ceramsite fracturing propping agent for oil and gas collection comprises the following steps:
(1) drying the municipal sludge, grinding the dried municipal sludge into powder, and then sieving the powder by a 400-mesh sieve to obtain sludge powder for later use.
(2) Respectively sieving the clay powder and the waste iron powder with a 400-mesh sieve to obtain clay powder and clay powder for later use.
(3) And mixing the sludge powder, the clay powder and the clay powder according to the weight ratio of 1.2: 1 part by weight: 0.35 part by weight of the components are uniformly mixed and then put into a granulator for granulation, and atomized water vapor is sprayed to ensure that the sludge powder forms spherical particles, wherein the average water content is 36%; the granules were dried at 140 ℃ for 2 hours to prepare a fracturing proppant precursor with an average diameter of about 0.6mm for use.
(4) And calcining the fracturing propping agent precursor at 1400 ℃ for 2 hours, and cooling the precursor to room temperature along with a furnace after the calcining is finished to obtain the ceramsite fracturing propping agent.
The performance indexes of the ceramsite fracturing propping agent prepared in each example are tested according to the specification of a standard SY/T5108-2006, and the results are shown in the following table.
Example number 1 2 3 4 5 6 7 8
Bulk Density (g/cm)3) 1.36 1.43 1.38 1.45 1.64 1.42 1.44 1.83
Apparent density (g/cm)3) 2.51 2.56 2.53 2.60 2.72 2.51 2.54 2.79
Breaking ratio (%) under a closing pressure of 52MPa 1.24 1.38 1.47 1.19 1.67 9.82 7.66 10.34
Percent breakage at a closure pressure of 69MPa (%) 3.88 3.62 3.80 3.74 4.03 13.17 9.31 13.73
Acid solubility (%) 4.38 3.86 4.22 3.95 4.19 4.63 7.57 7.08
From the test results, it can be seen that the core-shell fracturing propping agents prepared in examples 1 to 4 are not only low in density, but also have good compressive property, so that the purpose of reducing the density of the fracturing propping agent and maintaining the good compressive property of the fracturing propping agent is achieved, and the comprehensive properties of the fracturing propping agents prepared in examples 5 to 8 are obviously poorer than those of examples 1 to 4. The main reasons for this are: first, in embodiments 1 to 4, the characteristic that municipal sludge contains a large amount of organic matter components is utilized, the municipal sludge is used as an inner core of a fracturing propping agent, and the organic matter components in the inner core are fully volatilized and combusted after subsequent high-temperature long-time heating, so that the inner core is of a porous structure, and the integral density of the fracturing propping agent can be effectively reduced. Further, in the embodiments 1 to 4, clay and waste iron powder are used as raw materials, an inner coating layer with high iron powder content is prepared on the surface of the inner core, and the inner coating layer is calcined at a high temperature to form an iron-based ceramic inner coating layer, so that excellent pressure resistance can be provided for the fracturing propping agent. Finally, the process is carried out in a batch,
the surface of the inner coating layer is further coated with an outer coating layer in the embodiments 1-4, and the ceramic outer coating layer is formed after high-temperature calcination, so that the compression-resistant fracturing propping agent has good compression resistance, can protect the inner coating layer from being corroded, and prolongs the service life of the fracturing propping agent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (6)

1. A preparation method of a core-shell type ceramsite fracturing propping agent for oil and gas collection is characterized by comprising the following steps:
(1) grinding municipal sludge containing organic matters into powder, and then granulating and drying to obtain a kernel precursor; the diameter of the core precursor is controlled to be 0.5-0.8 mm;
(2) mixing clay and waste iron powder uniformly, adding water, and stirring uniformly to obtain inner cladding layer slurry; the proportion of the clay to the waste iron powder is 1 part by weight: 0.3 to 0.5 part by weight;
(3) mixing clay and water, and stirring uniformly to obtain outer coating layer slurry;
(4) immersing the kernel precursor into the slurry of the inner cladding layer to enable the outer surface of the kernel precursor to be uniformly coated with slurry, taking out the kernel precursor for drying, immersing the obtained particles into the slurry of the outer cladding layer again to enable the outer surface of the particles to be uniformly coated with slurry, taking out the particles for drying, putting the particles uniformly after the drying, calcining, and obtaining the ceramsite fracturing propping agent after the drying; the thickness of an inner cladding layer of the ceramsite fracturing propping agent is 0.3-0.5 mm, and the thickness of an outer cladding layer is 0.1-0.2 mm; the calcination temperature is 1350-1420 ℃, and the calcination time is 1-2 hours.
2. The preparation method of the core-shell ceramsite fracturing propping agent for oil and gas collection according to claim 1, wherein in the step (1), the water content of the granulated sludge particles is 35-40%.
3. The preparation method of the core-shell ceramsite fracturing propping agent for oil and gas collection according to claim 1, wherein in the step (1), the drying temperature is 120-150 ℃, and the drying time is 1.5-3 hours.
4. The preparation method of the core-shell type ceramsite fracturing propping agent for oil and gas collection according to claim 1, wherein in the step (2), the solid content of the slurry of the inner coating layer is 18-22%.
5. The preparation method of the core-shell type ceramsite fracturing propping agent for oil and gas collection according to claim 1, wherein in the step (3), the solid content of the slurry of the outer coating layer is 15-20%.
6. The preparation method of the core-shell ceramsite fracturing propping agent for oil and gas collection according to any one of claims 1 to 5, wherein in the step (4), the drying temperature is 80-90 ℃ and the drying time is 50-80 min.
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