CN114804844B - Method for comprehensively utilizing water-based rock debris through SiC template method - Google Patents

Method for comprehensively utilizing water-based rock debris through SiC template method Download PDF

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CN114804844B
CN114804844B CN202210263291.8A CN202210263291A CN114804844B CN 114804844 B CN114804844 B CN 114804844B CN 202210263291 A CN202210263291 A CN 202210263291A CN 114804844 B CN114804844 B CN 114804844B
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戚东涛
樊治海
蔡克
靳权
刘钊
常春丽
刘现伟
刘元煦
王君霞
沈立峰
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China Petroleum Engineering Materials Research Institute Co ltd
Henan Longdefu New Material Technology Research Institute Co ltd
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Henan Longdefu New Material Technology Research Institute Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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    • 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
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Abstract

The invention discloses a method for comprehensively utilizing water-based rock debris by a SiC template method. Taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing the water-based rock debris A, the water-based rock debris B and the SiC seed crystals, and ball-milling and uniformly mixing after mixing to obtain mixed powder; adding the mixed powder into a granulator for spray granulation to obtain a material with 20/140 meshes; drying the obtained material to obtain a spherical green body; and carrying out heat treatment on the spherical green body to obtain the high-strength novel propping agent. According to the technical scheme, the spherical mechanical material-novel propping agent with high strength is obtained through reasonable proportioning and normal pressure heat treatment. Therefore, the invention realizes the recycling of water-based rock debris, is beneficial to solving the problem of environmental pollution, and is expected to be used in the field of oil and gas exploitation.

Description

Method for comprehensively utilizing water-based rock debris through SiC template method
1. Technical field:
the invention belongs to the technical field of environmental protection and resource recycling, and particularly relates to a method for comprehensively utilizing water-based rock fragments through a SiC template method.
2. The background technology is as follows:
the water-based rock debris is a solid waste generated in petroleum exploration and development, and the main components of the water-based rock debris are shale, bentonite, lubricant, chloride and the like. If the generated water-based rock debris is not treated or is not treated properly, the generated water-based rock debris is easy to induce environmental pollution and endanger human health. In recent years, with the continuous importance of China on environmental problems, the reduction, environmental protection and recycling of solid wastes are required. Investigation shows that China does not have the capability of efficiently and industrially treating water-based rock debris on a large scale. Therefore, there is an urgent need to develop new approaches to the harmless and recycling treatment of water-based cuttings.
The chemical composition of the water-based rock debris contains Al 2 O 3 And SiO 2 These two components are the basic raw materials for producing corundum and mullite. The corundum and mullite can be prepared into structural materials such as fire resistance and the like by proper proportion. The SiC template method can induce the production of mullite and improve the mullite content, thereby improving the mechanical property of the material.
3. The invention comprises the following steps:
the invention aims to solve the technical problems that: according to the current processing state of the water-based rock debris, the invention provides a method for comprehensively utilizing the water-based rock debris by a SiC template method. According to the technical scheme, water-based rock scraps are used as raw materials, siC seed crystals are used as templates, and a spherical mechanical material-novel propping agent with high strength is obtained through normal-pressure heat treatment by reasonable proportioning. Therefore, the invention realizes the recycling of water-based rock debris, is beneficial to solving the problem of environmental pollution, and is expected to be used in the field of oil and gas exploitation.
In order to solve the problems, the invention adopts the following technical scheme:
the invention provides a method for comprehensively utilizing water-based rock fragments by a SiC template method, which comprises the following steps:
a. taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing the water-based rock debris A, the water-based rock debris B and the SiC seed crystals, and performing ball milling and mixing after mixing to obtain mixed powder;
b. adding the mixed powder obtained in the step a into a granulator for spray granulation to obtain a material with 20/140 meshes;
c. drying the material obtained in the step b to obtain a spherical green body;
d. and carrying out heat treatment on the obtained spherical green body, and obtaining the high-strength novel propping agent.
According to the method for comprehensively utilizing the water-based rock debris by the SiC template method, in the step a, the mass ratio of the water-based rock debris A to the water-based rock debris B to the SiC seed crystal is 100:10:2 to 10.
According to the method for comprehensively utilizing the water-based rock debris by the SiC template method, the water-based rock debris B in the step a contains CaO and MgO, and the mass fraction is more than 10 percent (the water-based rock debris A is a conventional general water-based rock debris, and the components of the water-based rock debris A are not specified).
According to the method for comprehensively utilizing the water-based rock fragments by the SiC template method, the ball milling and uniformly mixing in the step a is carried out by adopting a ball mill, wherein the rotating speed of the ball mill in the mixing process is 100-300 r/min, and the ball milling time is 12-48 h.
According to the method for comprehensively utilizing the water-based rock debris by the SiC template method, equipment adopted in the step b for spray granulation is a round pan granulator, and the frequency of the round pan granulator is 50Hz and the rotating speed of the round pan granulator is 20-30 r/min.
According to the method for comprehensively utilizing the water-based rock fragments by the SiC template method, in the step c, the drying is carried out by adopting a blast drying box, the drying temperature is 60-80 ℃, and the drying time is 12-48 h (the moisture content of the obtained product is less than or equal to 2 percent).
According to the method for comprehensively utilizing the water-based rock debris by the SiC template method, the specific process of the heat treatment in the step d is as follows: adding the spherical green body into a muffle furnace, heating to 1250 ℃ at a speed of 1-2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; and finally cooling to room temperature along with the furnace.
The invention has the positive beneficial effects that:
the water-based rock debris treated by the method is used as environmental pollutants and drilling waste, and provides a great challenge for environmental management and resource utilization. At present, the problems of secondary environmental pollution and low resource utilization rate can be caused by only carrying out treatment in the modes of landfill, incineration and brick making. If the water-based rock debris is used as raw materials or ingredients to prepare engineering materials with value and use value, the recycling of resources is expected, and the harm of the water-based rock debris to the environment is reduced to a certain extent. Usually, a certain composition design and a certain microscopic design are needed originally to prepare engineering materials with qualified quality, and particularly, a phase composition with high hardness and high toughness is needed to prepare a mechanical engineering material-fracturing propping agent. However, the inherent components of water-based cuttings are difficult to spontaneously achieve a high hardness, high toughness phase composition. Thus, there is a need to realize the preparation of fracturing proppants using water-based cuttings through microscopic design.
1. The technical proposal of the invention uses the larger length-diameter ratio of the SiC seed crystal to induce the inherent component Al of the water-based rock debris 2 O 3 And SiO 2 Formation of mullite phase 3Al during sintering 2 O 3 ·2SiO 2 . Because the mullite phase has the characteristics of high hardness and high toughness, the fracturing propping agent with high mechanical property (the breaking rate is 3.28%) is obtained.
2. The method for comprehensively utilizing the water-based rock debris by the SiC template method can realize the recycling of the water-based rock debris, is beneficial to solving the problem of environmental pollution, and is expected to be applied to the field of oil and gas exploitation.
In conclusion, according to the method, mullite is produced in an induction way through the action of the SiC seed crystal template, and the mullite content is improved, so that the mechanical property of the material is improved.
4. Description of the drawings:
figure 1 XRD pattern of the high strength novel proppant prepared in example 5 of the present invention.
FIG. 2 is an SEM image of a high strength novel proppant prepared according to example 5 of the present invention;
in the figure, M represents the mullite phase.
5. The specific embodiment is as follows:
the invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
In the following examples, the chemical components and contents of the water-based cuttings A and B are shown in Table 1.
TABLE 1 chemical compositions and contents of each of Water-based cuttings A and B
Figure BDA0003551585320000041
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Example 1 (comparative example):
a method for comprehensively utilizing water-based rock debris, which comprises the following detailed steps:
a. taking water-based rock debris A and water-based rock debris B as raw materials, mixing 100kg of water-based rock debris A and 10kg of water-based rock debris B by adopting a ball mill after mixing, wherein the rotation speed of the ball mill is 200r/min and the time is 24 hours in the mixing process, and obtaining mixed powder after ball milling and mixing uniformly;
b. adding the mixed powder obtained in the step a into a circular pan granulator for spray granulation, wherein the frequency of the circular pan granulator is 50Hz, and the rotating speed of the circular pan granulator is 25-30 r/min; granulating to obtain a material with the granularity of 20/140 meshes;
c. drying the material obtained in the step b by adopting a blast drying oven at the drying temperature of 80 ℃ until the water content of the obtained product is less than or equal to 2%, so as to obtain a spherical green body with the thickness of 0.8 cm;
d. adding the obtained spherical green body into a muffle furnace for heat treatment, heating to 1250 ℃ at a speed of 2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; finally, cooling to room temperature along with the furnace to obtain a sample No. 1, wherein the performance of the sample is shown in Table 2.
Example 2:
the invention relates to a method for comprehensively utilizing water-based rock fragments by a SiC template method, which comprises the following detailed steps:
a. taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing 100kg of water-based rock debris A, 10kg of water-based rock debris B and 2kg of SiC seed crystals by adopting a ball mill after mixing, wherein the rotation speed of the ball mill is 260r/min and the ball milling time is 20h in the mixing process, and obtaining mixed powder after ball milling and mixing uniformly;
b. adding the mixed powder obtained in the step a into a circular pan granulator for spray granulation, wherein the frequency of the circular pan granulator is 50Hz, and the rotating speed of the circular pan granulator is 20-25 r/min; granulating to obtain a material with the granularity of 20/140 meshes;
c. drying the material obtained in the step b by adopting a blast drying oven at the drying temperature of 70 ℃ until the water content of the obtained product is less than or equal to 2%, so as to obtain a spherical green body with the thickness of 0.8 cm;
d. adding the obtained spherical green body into a muffle furnace for heat treatment, heating to 1250 ℃ at a speed of 2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; finally cooling to room temperature along with the furnace to obtain the high-strength novel proppant with the number of 2# and the performance shown in Table 2.
Example 3:
the invention relates to a method for comprehensively utilizing water-based rock fragments by a SiC template method, which comprises the following detailed steps:
a. taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing 100kg of water-based rock debris A, 10kg of water-based rock debris B and 4kg of SiC seed crystals by adopting a ball mill after mixing, wherein the rotating speed of the ball mill is 180r/min and the ball milling time is 32h in the mixing process, and obtaining mixed powder after ball milling and mixing uniformly;
b. adding the mixed powder obtained in the step a into a circular pan granulator for spray granulation, wherein the frequency of the circular pan granulator is 50Hz, and the rotating speed of the circular pan granulator is 20-25 r/min; granulating to obtain a material with the granularity of 20/140 meshes;
c. drying the material obtained in the step b by adopting a blast drying oven at the drying temperature of 60 ℃ until the water content of the obtained product is less than or equal to 2%, so as to obtain a spherical green body with the thickness of 0.8 cm;
d. adding the obtained spherical green body into a muffle furnace for heat treatment, heating to 1250 ℃ at a speed of 2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; finally cooling to room temperature along with the furnace to obtain the high-strength novel proppant with the number of 3# and the performance shown in Table 2.
Example 4:
the invention relates to a method for comprehensively utilizing water-based rock fragments by a SiC template method, which comprises the following detailed steps:
a. taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing 100kg of water-based rock debris A, 10kg of water-based rock debris B and 6kg of SiC seed crystals by adopting a ball mill after mixing, wherein the rotating speed of the ball mill is 260r/min and the ball milling time is 20h in the mixing process, and obtaining mixed powder after ball milling and mixing uniformly;
b. adding the mixed powder obtained in the step a into a circular pan granulator for spray granulation, wherein the frequency of the circular pan granulator is 50Hz, and the rotating speed of the circular pan granulator is 20-25 r/min; granulating to obtain a material with the granularity of 20/140 meshes;
c. drying the material obtained in the step b by adopting a blast drying oven at the drying temperature of 80 ℃ until the water content of the obtained product is less than or equal to 2%, so as to obtain a spherical green body with the thickness of 0.8 cm;
d. adding the obtained spherical green body into a muffle furnace for heat treatment, heating to 1250 ℃ at a speed of 2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; finally cooling to room temperature along with the furnace to obtain the high-strength novel proppant with the number of 4# and the performance shown in Table 2.
Example 5:
the invention relates to a method for comprehensively utilizing water-based rock fragments by a SiC template method, which comprises the following detailed steps:
a. taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing 100kg of water-based rock debris A, 10kg of water-based rock debris B and 8kg of SiC seed crystals by adopting a ball mill after mixing, wherein the rotation speed of the ball mill is 220r/min and the ball milling time is 36h in the mixing process, and obtaining mixed powder after ball milling and mixing uniformly;
b. adding the mixed powder obtained in the step a into a circular pan granulator for spray granulation, wherein the frequency of the circular pan granulator is 50Hz, and the rotating speed of the circular pan granulator is 20-25 r/min; granulating to obtain a material with the granularity of 20/140 meshes;
c. drying the material obtained in the step b by adopting a blast drying oven at the drying temperature of 80 ℃ until the water content of the obtained product is less than or equal to 2%, so as to obtain a spherical green body with the thickness of 0.8 cm;
d. adding the obtained spherical green body into a muffle furnace for heat treatment, heating to 1250 ℃ at a speed of 2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; finally cooling to room temperature along with the furnace to obtain the high-strength novel proppant with the number of 5# and the performance shown in Table 2.
Example 6:
the invention relates to a method for comprehensively utilizing water-based rock fragments by a SiC template method, which comprises the following detailed steps:
a. taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing 100kg of water-based rock debris A, 10kg of water-based rock debris B and 10kg of SiC seed crystals by adopting a ball mill after mixing, wherein the rotation speed of the ball mill is 200r/min and the ball milling time is 26h in the mixing process, and obtaining mixed powder after ball milling and mixing uniformly;
b. adding the mixed powder obtained in the step a into a circular pan granulator for spray granulation, wherein the frequency of the circular pan granulator is 50Hz, and the rotating speed of the circular pan granulator is 20-25 r/min; granulating to obtain a material with the granularity of 20/140 meshes;
c. drying the material obtained in the step b by adopting a blast drying oven at the drying temperature of 70 ℃ until the water content of the obtained product is less than or equal to 2%, so as to obtain a spherical green body with the thickness of 0.8 cm;
d. adding the obtained spherical green body into a muffle furnace for heat treatment, heating to 1250 ℃ at a speed of 2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; finally cooling to room temperature along with the furnace to obtain the high-strength novel proppant with the number of 6# and the performance shown in Table 2.
TABLE 2 various indices of the products obtained in examples 1 to 6
Figure BDA0003551585320000081
As shown by the experimental data results in Table 2, the crushing rates of the No. 1 and No. 2 samples do not meet the requirements of the standards (SY/T5108-2014 and Q/SY 17025-2019, and the crushing rate is less than or equal to 9%). Along with the continuous increase of the adding amount of SiC, the crushing rate is reduced, and then the crushing rate is increased until the crushing rate of the No. 5 sample is the lowest, and the requirement of the standard on the crushing rate is met. Considering practicality and economy, the preferable dosage of SiC is 8 parts, namely the optimal mass ratio of water-based rock debris A to water-based rock debris B serving as raw materials to SiC seed crystal is 100:10:8.
therefore, the technical scheme of the invention can realize the comprehensive utilization of water-based rock debris through the action of the SiC template.

Claims (3)

1. The method for comprehensively utilizing the water-based rock fragments by the SiC template method is characterized by comprising the following steps of:
a. taking water-based rock debris A and water-based rock debris B as raw materials and SiC seed crystals as templates, mixing the water-based rock debris A, the water-based rock debris B and the SiC seed crystals, and performing ball milling and mixing after mixing to obtain mixed powder;
the mass ratio of the water-based rock debris A to the water-based rock debris B to the SiC seed crystal is 100:10:2 to 10; the water-based rock debris B contains CaO and MgO, and the mass fractions of the CaO and MgO are all more than 10%;
b. adding the mixed powder obtained in the step a into a granulator for spray granulation to obtain a material with 20/140 meshes;
the equipment adopted by the spray granulation is a round pan granulator, wherein the frequency of the round pan granulator is 50Hz, and the rotating speed is 20-30 r/min;
c. drying the material obtained in the step b to obtain a spherical green body;
d. carrying out heat treatment on the spherical green body to obtain a product high-strength propping agent;
the specific process of the heat treatment is as follows: adding the spherical green body into a muffle furnace, heating to 1250 ℃ at a speed of 1-2 ℃/min, and sintering for 5min at the temperature; then cooling at a speed of 5 ℃/min, and preserving heat for 2 hours under the condition of cooling to 1200 ℃; and finally cooling to room temperature along with the furnace.
2. The method for comprehensively utilizing water-based rock debris by a SiC template method according to claim 1, wherein: and (c) ball milling and uniformly mixing in the step a, wherein a ball mill is adopted for mixing, the rotating speed of the ball mill in the mixing process is 100-300 r/min, and the ball milling time is 12-48 h.
3. The method for comprehensively utilizing water-based rock debris by a SiC template method according to claim 1, wherein: and c, drying in the step of drying by adopting a blast drying oven, wherein the drying temperature is 60-80 ℃ and the drying time is 12-48 h.
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US9382468B2 (en) * 2009-12-30 2016-07-05 Schlumberger Technology Corporation Hydraulic fracturing proppant containing inorganic fibers
CN103253981B (en) * 2013-04-25 2015-04-15 南昌大学 Preparation method of mullite/silicon carbide complex-phase foamed ceramic
CN106362675A (en) * 2016-10-10 2017-02-01 四川奎能环保科技有限公司 Resource utilization method of water-based rock debris
CN110395993B (en) * 2019-07-25 2021-10-01 哈尔滨工业大学 Preparation method of nano SiC modified nano-structure mullite powder feed for plasma spraying
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