CN110628411B - Low-density petroleum fracturing propping agent and preparation method thereof - Google Patents

Low-density petroleum fracturing propping agent and preparation method thereof Download PDF

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CN110628411B
CN110628411B CN201910903611.XA CN201910903611A CN110628411B CN 110628411 B CN110628411 B CN 110628411B CN 201910903611 A CN201910903611 A CN 201910903611A CN 110628411 B CN110628411 B CN 110628411B
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CN110628411A (en
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司峻山
贺永利
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Datang Tongzhou Technology Co Ltd
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    • C09K8/80Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open

Abstract

The invention discloses a low-density petroleum fracturing propping agent and a preparation method thereof, and belongs to the technical field of petroleum fracturing propping agents. The low-density petroleum fracturing propping agent is prepared from light-burned bauxite, bentonite, light-burned magnesium powder, manganese powder, overburning recycled powder, silica fume and low-alumina fly ash. The invention also discloses a preparation method of the low-density petroleum fracturing propping agent, which comprises the steps of proportioning, pulping, homogenizing, drying, granulating and screening, and the calcined blank balls are crushed and then used as calcined recycling powder, so that the problem of raw material waste is reduced, the density of the product is reduced, the stability and strength of the product are improved, the resource utilization is realized, and the large-scale production is facilitated.

Description

Low-density petroleum fracturing propping agent and preparation method thereof
Technical Field
The invention relates to the technical field of petroleum fracturing propping agents, in particular to a low-density petroleum fracturing propping agent and a preparation method thereof.
Background
When the petroleum and natural gas deep well is exploited, after the high-closure-pressure low-permeability deposit is subjected to fracturing treatment, the petroleum-containing rock stratum is cracked, the petroleum and gas are collected from a channel formed by the cracks, at the moment, the fluid is required to be injected into the rock base layer so as to exceed the pressure of the fracture strength of the stratum, the rock stratum around the shaft is cracked, a channel with high laminar flow capacity is formed, and in order to keep the cracks formed after fracturing open, the petroleum and gas products can smoothly pass through the channel.
At present, the types of proppants commonly used for fracture acidizing in the oil and gas industry are many, but only quartz sand and artificial sintered ceramsite have good comprehensive performance. The quartz sand has the advantages of low cost and good flow conductivity, but has poor compressive strength and low sphericity which is generally about 21-35 MPa, the application range is limited to a shallow well, the quartz sand is not suitable for a deep well with high closing pressure, bauxite is used as a main raw material for manufacturing the quartz sand, the production is stopped in many places by using sintered ceramsite proppant plants which take bauxite as the main raw material under the influence of national environmental protection policies, and the product cannot meet the market; the traditional artificial sintered ceramsite has high compressive strength and good flow conductivity, but has high cost. With the development of fracturing technology, which is forced to be environmentally friendly and economical, oil and gas fields are in urgent need of a petroleum proppant product with high strength, low density and low cost.
In addition, about 1% of over-burnt unqualified proppant waste materials are generated in the production process of the existing petroleum fracturing proppant, the performance of the over-burnt petroleum fracturing proppant is low, and the conventional treatment mode of the over-burnt petroleum fracturing proppant is to carry out landfill treatment on the over-burnt petroleum fracturing proppant, so that the problem of resource waste exists.
In view of the above, there is a need to provide a new low density oil fracturing proppant to overcome the deficiencies of the prior art.
Disclosure of Invention
One of the objects of the present invention is to provide a low density petroleum fracturing proppant. The method adopts industrial solid wastes of a power plant as main raw materials to prepare the low-density petroleum fracturing propping agent, and simultaneously has low breaking ground under closed pressure, so that the materials in the preparation process are reasonably utilized, and the resource loss is reduced.
The technical scheme for solving the technical problems is as follows:
the invention provides a low-density petroleum fracturing propping agent which is prepared from the following components:
4 to 6 percent of light-burned bauxite, 6 to 8 percent of bentonite, 0.8 to 1.2 percent of manganese powder, 0.8 to 1.2 percent of light-burned magnesium powder, 0.4 to 0.6 percent of silica fume, 0 to 0.5 percent of over-burned recycled powder and the balance of low-aluminum fly ash.
The principle of the invention is as follows:
in the present invention, light-burned bauxite is used as an aluminum supplement; bentonite is used as an adhesive; manganese powder and light-burned magnesium powder are used as fluxing agents; silicon powder is used as a thermal shock resistant agent; overburning the recycled powder as aggregate; the ceramsite proppant adopting the low-aluminum fly ash as the raw material has low density, strength far higher than that of quartz sand, sphericity better than that of bauxite ceramsite proppant, corrosion resistance, high temperature resistance, high pressure resistance and cost far lower than that of bauxite proppant, so that the ceramsite proppant has good market prospect and belongs to a green and environment-friendly product supported by great strength in China.
The volume density of the low-density petroleum fracturing propping agent is 1.28g/cm3~1.40g/cm3Apparent density of 2.65g/cm3~2.80g/cm3The breaking rate under 28Mpa closing pressure, 35Mpa closing pressure and 40Mpa closing pressure is less than 3%. While the prior art for oil fracturing proppantsThe bulk density is 1.45g/cm3~1.60g/cm3Apparent density of 2.70g/cm3~2.80g/cm3The breaking rate under 28Mpa closing pressure, 35Mpa closing pressure and 40Mpa closing pressure is less than 9%. Compared with the prior art, under the condition that the apparent density is basically unchanged, the volume density of the low-density petroleum fracturing propping agent is reduced by 10% at most compared with the prior art, namely the open gap of the low-density petroleum propping agent is improved, the smoothness of oil gas products passing through the petroleum fracturing propping agent is increased, and then under the same closing pressure, the breaking rate of the low-density petroleum fracturing propping agent under the closing pressure of 28MPa, the closing pressure of 35MPa and the closing pressure of 40MPa is not more than 33% of the breaking rate of the prior art.
The invention has the beneficial effects that: compared with the prior art, the invention takes the low-alumina fly ash as the raw material and the over-burnt recycled powder as the aggregate, under the condition that the apparent density is basically unchanged, the volume density is reduced by 10 percent at most compared with the prior art, the smoothness of a petroleum product passing through the petroleum proppant is effectively improved, the stability and the strength of the proppant can be enhanced, the breakage rate under the closing pressure is lower than that of the prior art, and the generation of waste materials is reduced.
On the basis of the technical scheme, the invention can be further improved as follows.
Preferably, in the light-burned bauxite, Al2O3The mass percentage content of the compound is 70-75 percent; in the bentonite, the mass percentage of the montmorillonite is 85-90%; in the low-aluminum fly ash, Al2O333.08 to 50.10 percent of SiO235.10 to 42.67 percent of Fe2O3The mass percentage of the CaO is 1.8-4.0%, and the mass percentage of the CaO is 8-12%; the light-burned bauxite, the bentonite, the manganese powder, the light-burned magnesium powder, the low-aluminum fly ash and the silica fume are sieved by a 200-mesh sieve.
The invention also aims to provide a preparation method of the low-density petroleum fracturing propping agent. The preparation method is simple, easy to operate, wide in market prospect and suitable for large-scale production.
The technical scheme for solving the technical problems is as follows: a preparation method of a low-density petroleum fracturing propping agent comprises the following steps:
s1: adding the low-aluminum fly ash crude product into a straight tube ball mill, removing large materials, and sieving with a 200-300-mesh sieve to obtain low-aluminum fly ash ball milled powder;
s2: weighing the following raw materials in percentage by mass: 4 to 6 percent of light-burned bauxite, 6 to 8 percent of bentonite, 0.8 to 1.2 percent of manganese powder, 0.8 to 1.2 percent of light-burned magnesium powder, 0.4 to 0.6 percent of silica fume, 0 to 0.5 percent of over-burned recycled powder from S6 and the balance of the low-aluminum fly ash ball-milled powder obtained in the step S1 are mixed and homogenized to obtain mixed powder, and then the mixed powder is mixed with water for pulping to obtain slurry;
s3: grinding the slurry obtained in the step S2 to 600-800 meshes in a ceramic ball mill to obtain superfine powder slurry, drying the superfine powder slurry in a dryer, drying 5-15 wt% of the superfine powder slurry to obtain dry powder with the moisture content of less than or equal to 2.0%, and drying the rest superfine powder slurry to obtain semi-wet powder with the moisture content of 7.5-8.5%;
s4: adding water to spray the dry powder and the semi-wet powder obtained in the step S3 in a granulator, granulating and forming to obtain semi-finished blank balls, wherein the granulation and forming time is 1.4-1.6 h, drying the semi-finished blank balls, classifying and screening according to particle size to respectively obtain qualified blank balls, large-particle blank balls and small-particle blank balls, crushing the large-particle blank balls to 600-800 meshes, mixing with the semi-wet powder obtained in the step S3, and returning the small-particle blank balls to the granulator for re-granulation;
s5, heating and sintering the qualified blank balls obtained in the step S4 in an automatic high-temperature resistance furnace or a rotary kiln by a program, wherein the sintering temperature is 1350 +/-20 ℃, the sintering heat preservation time is 0.8-1.2 h, and after the sintering is finished, naturally cooling to the normal temperature for 5h to obtain the sintered blank balls;
s6, screening the fired blank balls obtained in the step S5 step by step, firstly screening out under-fired blank balls through a color screening machine, then screening out over-fired blank balls through particle size, finally obtaining finished product blank balls, returning the under-fired blank balls to the step S5 for re-firing, punching and crushing the over-fired blank balls under 27-29 MPa, then vibrating and screening to obtain powder, and crushing the powder into 600-800 meshes through an ultrafine grinder as the over-fired recycled powder in the step S2;
and S7, grading and screening the screened finished product blank balls through a standard screen to obtain the low-density petroleum fracturing propping agent.
The invention has the beneficial effects that: according to the invention, the superfine powder slurry obtained by the ceramic ball mill can effectively homogenize and crush the mixed powder, thereby being beneficial to forming; the dry materials are added to adjust the growth speed of blank ball forming, so that the influence on the final product caused by the too fast blank ball forming can be avoided; the over-sintered blank balls are crushed and then recycled to the ingredients to serve as aggregate, so that the generation of waste in the technical process can be reduced, various materials are recycled, the large-scale production is facilitated, and the performance of the prepared petroleum fracturing propping agent meets the technical standard of SY/T5108-2014.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the volume ratio of the mixed powder and the water mixed for pulping in the step S2 is 1: 1.5.
The beneficial effects of adopting the further scheme are as follows: can effectively disperse the mixed powder, and is convenient for subsequent ball milling.
Further, in step S3, the ultrafine powder slurry has a passing rate of 90% to 100% after passing through a 600-mesh water screen.
The beneficial effects of adopting the further scheme are as follows: therefore, the solid powder in the superfine powder slurry can reach the size, and the petroleum propping agent can reduce the volume density.
Further, in step S4, when the dry powder and the semi-wet powder are subjected to water spray granulation and molding in the granulator, the mass percentage of the dry powder is 0% to 10%, and the mass percentage of the semi-wet powder is 90% to 100%.
The beneficial effects of adopting the further scheme are as follows: the rotating speed and the water mist stirring change can influence the growth speed of blank ball forming, and proper dry powder is added, so that the blank ball can be formed in proper size in relatively stable time, and the blank ball forming of large particles or small particles can be reduced.
Further, the qualified green pellets are green pellets screened by any one of a standard screen of 20 to 40 mesh, a standard screen of 30 to 50 mesh and a standard screen of 40 to 60 mesh, the large-particle green pellets are green pellets that cannot be screened by the upper limit of one of the standard screens, and the small-particle green pellets are green pellets that can be screened by the lower limit of one of the standard screens.
The beneficial effects of adopting the further scheme are as follows: unqualified products in the semi-finished blank balls can be effectively removed through screening, so that the particle size in the sintering process is in a reasonable range, the unqualified products are prevented from entering the sintering step, and the waste of sintering energy is reduced.
Further, in step S4, the semi-finished blank ball is dried until the moisture content is less than 2% and the drying temperature is 103-107 ℃.
The beneficial effects of adopting the further scheme are as follows: the strength of the semi-finished blank balls can be effectively improved after the semi-finished blank balls are dried, and the damage of the screen to the semi-finished blank balls caused by low strength when the semi-finished blank balls are subjected to grading screening is avoided.
Further, in step S5, the temperature-programmed rate is 3 ℃/min to 5 ℃/min, and the temperature-programmed time is 5.8h to 6.2 h.
The beneficial effects of adopting the further scheme are as follows: the temperature difference between the center of the blank ball and the outer wall of the blank ball in the heating process can be small by adopting a temperature programming mode, so that the blank ball is convenient to fire.
Further, in step S6, the color screening machine marks the color of the qualified pellet as red, marks the color of the qualified pellet as green, the color screening machine screens out the pellet marked as green as the under-fired pellet, the pellet marked as green is screened out by the color screening machine as the pellet, the pellet subjected to over-firing is screened out by a 20-mesh screen, and the pellet subjected to over-firing obtained after screening is primarily crushed by a jaw crusher before being crushed by the punching.
The beneficial effects of adopting the further scheme are as follows: the jaw crusher can damage a flaky or blocky structure formed by overburning to form a small-particle structure, so that the structure is more favorable for stamping and crushing, and overburning blank balls can be effectively crushed in multiple layers, so that powder with the particle size higher than 600 meshes can be formed for batching; the color screening machine can screen out the unfired blank balls with poor chromaticity and re-sinter the unfired blank balls, so that the total yield of the qualified blank balls is improved.
Drawings
Fig. 1 is a flow chart of a method of making a low density petroleum fracturing proppant of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
The low-density petroleum fracturing propping agent is prepared from the following components:
4 to 6 percent of light-burned bauxite, 6 to 8 percent of bentonite, 0.8 to 1.2 percent of manganese powder, 0.8 to 1.2 percent of light-burned magnesium powder, 0.4 to 0.6 percent of silica fume, 0 to 0.5 percent of over-burned recycled powder and the balance of low-aluminum fly ash.
Wherein, in the light-burned bauxite, Al2O3The mass percentage content of the compound is 70 percent; in the bentonite, the mass percentage of montmorillonite is 85%; in the low-aluminum fly ash, Al2O3Is 36.52 percent by mass, SiO238.56% by mass of Fe2O3The mass percentage of the CaO is 4.05 percent, and the mass percentage of the CaO is 10.35 percent; the light-burned bauxite, the bentonite, the manganese powder, the light-burned magnesium powder, the low-aluminum fly ash and the silica fume are sieved by a 200-mesh sieve, and the passing rate is 99%.
As shown in fig. 1, the preparation method of the low-density petroleum fracturing proppant comprises the following steps:
s1: adding the industrial solid waste low-alumina fly ash crude product which takes quasi-Geer coal as power generation fuel by Inmunogu Datang International tokto power generation Limited company into a straight tube ball mill, removing large materials, and sieving with a 200-300-mesh sieve to obtain low-alumina fly ash ball milled powder;
s2: weighing the following raw materials in percentage by mass: mixing 5.0Kg of light calcined alumina, 7.0Kg of bentonite, 1.0Kg of manganese powder, 1.0Kg of light calcined magnesium powder, 0.50Kg of silica fume, 0.300Kg of overburning recycled powder obtained in the step S6, 85.2Kg of the mixture and the balance of low-alumina fly ash ball-milled powder obtained in the step S1, homogenizing the mixture to obtain mixed powder, mixing the mixed powder with water for pulping, wherein the volume ratio of the mixed powder to the water for pulping is 1:1.5, and obtaining slurry;
s3: grinding the slurry obtained in the step S2 to 600-800 meshes in a ceramic ball mill, wherein the passing rate of the superfine powder slurry after passing through a 600-mesh water sieve is 90-100%, so as to obtain superfine powder slurry, drying the superfine powder slurry in a dryer, then drying 10% of the superfine powder slurry to prepare dry powder with the moisture content of less than or equal to 2.0%, and drying the rest superfine powder slurry to prepare semi-wet powder with the moisture content of 8.0%;
s4: adding water spray to the dry powder and the semi-wet powder obtained in the step S3 in a granulator, granulating and forming, wherein when the dry powder and the semi-wet powder are subjected to water spray granulation and forming in the granulator, the mass percentage of the dry powder is 0-10%, the mass percentage of the semi-wet powder is 90-100%, the addition amount of the dry powder is adjusted according to the rotating speed of the granulator and the water addition amount in the water spray process, the aim is to keep the granulation and forming time at 1.5h to obtain semi-finished product blank balls, the granulation and forming time is 1.5h, the semi-finished product blank balls are dried until the water content is less than 2%, the drying temperature is 105 ℃, then the dried products are classified and screened according to particle size to respectively obtain qualified blank balls, large-particle blank balls and small-particle blank balls, and the qualified blank balls are sieved by a 20-40-mesh standard screen, Sieving the large-particle blank balls by any one of a 30-50-mesh standard sieve and a 40-60-mesh standard sieve to obtain blank balls, wherein the large-particle blank balls are blank balls which cannot be sieved by an upper limit sieve of one of the standard sieves, the small-particle blank balls are blank balls which can be sieved by a lower limit sieve of one of the standard sieves, crushing the large-particle blank balls to 600-800 meshes, mixing the crushed large-particle blank balls with the semi-wet powder in the step S3, and returning the small-particle blank balls to the granulator for re-granulation;
s5, performing temperature programmed sintering on the qualified blank balls obtained in the step S4 in an automatic high-temperature resistance furnace or a rotary kiln, wherein the sintering temperature is 1350 ℃, the sintering heat preservation time is 1.0h, in the step S5, the temperature rising rate of the temperature programmed sintering is 3 ℃/min to 5 ℃/min, the temperature rising rate is 5 ℃/min when the temperature is lower than 1000 ℃, the temperature rising rate is gradually reduced to 3 ℃/min when the temperature rises from 1000 ℃ to 1300 ℃, the time of the temperature programmed sintering is 5.8h to 6.2h, after the sintering is finished, naturally cooling to the normal temperature, and the cooling time is 5h, so that the sintered blank balls are obtained;
s6, screening the fired blank balls obtained in the step S5 step by step, firstly, screening out under-fired blank balls through a color screening machine, wherein the color screening machine marks the colors of the qualified blank balls as red, marks the colors of the qualified blank balls, which are 30% lower than the chroma of the qualified blank balls, as green, the color screening machine screens out the under-fired blank balls marked as green, and returning the obtained under-fired blank balls to the step S5 for re-firing; screening out fired blank balls through the particle size, screening out the fired blank balls through a 20-mesh screen, preliminarily crushing the screened fired blank balls through a jaw crusher before the fired blank balls are subjected to stamping and crushing, stamping and crushing the fired blank balls under 28MPa, vibrating and screening to obtain powder, and crushing the powder into 600-800 meshes through an ultrafine crusher to obtain the fired recycled powder in the step S2; finally, obtaining a finished product blank ball;
and S7, grading and screening the screened finished product blank balls through a standard screen to obtain the low-density petroleum fracturing propping agent.
According to the SY/T5108-2014 standard, the volume density, the apparent density and the fracture degree under different specifications of closed pressure of the 20-40-mesh petroleum fracturing propping agent are measured, and the result is as follows: bulk density 1.34g/cm3Apparent density2.80g/cm3(ii) a Under the closing pressure of 28MPa, the breaking rate of the 20-40 mesh (850-425 mu m) petroleum fracturing propping agent is less than 1.67 percent, and the standard of SY/T5108-.
The petroleum fracturing propping agent with the granularity of 30-50 meshes (600-300 mu m) is prepared according to the proportion, and the volume density, the apparent density and the breaking degree under different specifications of closing pressure of the petroleum fracturing propping agent are measured according to the SY/T5108-2014 standard, and the result is as follows: bulk density 1.30g/cm3Apparent density 2.78g/cm3(ii) a Under the closing pressure of 35MPa, the breaking rate of the 30-50 mesh (600-300 mu m) petroleum fracturing propping agent is less than 1.75 percent, and the standard of SY/T5108-2014 is less than or equal to 9.0 percent.
The petroleum fracturing propping agent with the granularity of 40-60 meshes (425-250 mu m) is prepared according to the proportion, and the volume density, the apparent density and the breaking degree under different specifications of closing pressure of the petroleum fracturing propping agent are measured according to the SY/T5108-2014 standard, and the result is as follows: bulk density 1.31g/cm3Apparent density 2.75g/cm3(ii) a Under the closing pressure of 28MPa, the breakage rate of the 40-60 mesh (425-250 mu m) petroleum fracturing propping agent is less than 1.98 percent, and the standard of SY/T5108-.
Example 2
The low-density petroleum fracturing propping agent is prepared from the following components:
4 to 6 percent of light-burned bauxite, 6 to 8 percent of bentonite, 0.8 to 1.2 percent of manganese powder, 0.8 to 1.2 percent of light-burned magnesium powder, 0.4 to 0.6 percent of silica fume, 0 to 0.5 percent of over-burned recycled powder and the balance of low-aluminum fly ash.
Wherein, in the light-burned bauxite, Al2O3The mass percentage content of the compound is 70 percent; in the bentonite, the mass percentage of montmorillonite is 85%; in the low-aluminum fly ash, Al2O3Is 36.52 percent by mass, SiO238.56% by mass of Fe2O3The mass percentage of the CaO is 4.05 percent, and the mass percentage of the CaO is 10.35 percent; the light-burned bauxite, the bentonite, the manganese powder, the light-burned magnesium powder, the low-aluminum fly ash and the silica fume are sieved by a 200-mesh sieve, and the passing rate is 99 percent。
As shown in fig. 1, the preparation method of the low-density petroleum fracturing proppant comprises the following steps:
s1: adding the industrial solid waste low-alumina fly ash crude product which takes quasi-Geer coal as power generation fuel by Inmunogu Datang International tokto power generation Limited company into a straight tube ball mill, removing large materials, and sieving with a 200-300-mesh sieve to obtain low-alumina fly ash ball milled powder;
s2: weighing the following raw materials in percentage by mass: 4.0Kg of light calcined alumina, 6.0Kg of bentonite, 1.0Kg of manganese powder, 1.0Kg of light calcined magnesia powder, 0.50Kg of silica fume, 0.300Kg of overburning recycled powder and 87.2Kg of low-alumina fly ash ball-milled powder obtained in the step S1 are mixed and homogenized to obtain mixed powder, and then the mixed powder is mixed with water for pulping, wherein the volume ratio of the mixed powder to the water for pulping is 1:1.5, so as to obtain slurry;
s3: grinding the slurry obtained in the step S2 to 600-800 meshes in a ceramic ball mill, wherein the passing rate of the superfine powder slurry after passing through a 600-mesh water sieve is 90-100%, so as to obtain superfine powder slurry, drying the superfine powder slurry in a dryer, then drying 10% of the superfine powder slurry to prepare dry powder with the moisture content of less than or equal to 2.0%, and drying the rest superfine powder slurry to prepare semi-wet powder with the moisture content of 8.0%;
s4: adding water spray to the dry powder and the semi-wet powder obtained in the step S3 in a granulator, granulating and forming, wherein when the dry powder and the semi-wet powder are subjected to water spray granulation and forming in the granulator, the mass percentage of the dry powder is 0-10%, the mass percentage of the semi-wet powder is 90-100%, the addition amount of the dry powder is adjusted according to the rotating speed of the granulator and the water addition amount in the water spray process, the aim is to keep the granulation and forming time at 1.5h to obtain semi-finished product blank balls, the granulation and forming time is 1.5h, the semi-finished product blank balls are dried until the water content is less than 2%, the drying temperature is 105 ℃, then the dried products are classified and screened according to particle size to respectively obtain qualified blank balls, large-particle blank balls and small-particle blank balls, and the qualified blank balls are sieved by a 20-40-mesh standard screen, Sieving the large-particle blank balls by any one of a 30-50-mesh standard sieve and a 40-60-mesh standard sieve to obtain blank balls, wherein the large-particle blank balls are blank balls which cannot be sieved by an upper limit sieve of one of the standard sieves, the small-particle blank balls are blank balls which can be sieved by a lower limit sieve of one of the standard sieves, crushing the large-particle blank balls to 600-800 meshes, mixing the crushed large-particle blank balls with the semi-wet powder in the step S3, and returning the small-particle blank balls to the granulator for re-granulation;
s5, performing temperature programmed sintering on the qualified blank balls obtained in the step S4 in an automatic high-temperature resistance furnace or a rotary kiln, wherein the sintering temperature is 1350 ℃, the sintering heat preservation time is 1.0h, in the step S5, the temperature rising rate of the temperature programmed sintering is 3 ℃/min to 5 ℃/min, the temperature rising rate is 5 ℃/min when the temperature is lower than 1000 ℃, the temperature rising rate is gradually reduced to 3 ℃/min when the temperature rises from 1000 ℃ to 1300 ℃, the time of the temperature programmed sintering is 5.8h to 6.2h, after the sintering is finished, naturally cooling to the normal temperature, and the cooling time is 5h, so that the sintered blank balls are obtained;
s6, screening the fired blank balls obtained in the step S5 step by step, firstly, screening out under-fired blank balls through a color screening machine, wherein the color screening machine marks the colors of the qualified blank balls as red, marks the colors of the qualified blank balls, which are 30% lower than the chroma of the qualified blank balls, as green, the color screening machine screens out the under-fired blank balls marked as green, and returning the obtained under-fired blank balls to the step S5 for re-firing; screening out fired blank balls through the particle size, screening out the fired blank balls through a 20-mesh screen, preliminarily crushing the screened fired blank balls through a jaw crusher before the fired blank balls are subjected to stamping and crushing, stamping and crushing the fired blank balls under 28MPa, vibrating and screening to obtain powder, and crushing the powder into 600-800 meshes through an ultrafine crusher to obtain the fired recycled powder in the step S2; finally, obtaining a finished product blank ball;
and S7, classifying and screening the screened finished product blank balls through a standard screen to obtain the petroleum fracturing propping agent with the mesh number of 20-40 meshes, and obtaining the low-density petroleum fracturing propping agent.
According to the SY/T5108-2014 standard, the measurement is carried out for 20-40 meshesThe volume density, apparent density and the degree of fracture under different specifications of closing pressure of the petroleum fracturing propping agent have the following results: bulk density 1.34g/cm3Apparent density of 2.80g/cm3(ii) a Under the closing pressure of 28MPa, the breaking rate of the 20-40 mesh (850-425 mu m) petroleum fracturing propping agent is less than 2.82%, and the SY/T5108-2014 standard is less than or equal to 9.0%.
The petroleum fracturing propping agent with the granularity of 30-50 meshes (425-250 mu m) is prepared according to the proportion, and the volume density, the apparent density and the breaking degree under different specifications of closing pressure of the petroleum fracturing propping agent are measured according to the SY/T5108-2014 standard, and the result is as follows: bulk density 1.37g/cm3Apparent density 2.78g/cm3(ii) a Under the closing pressure of 35MPa, the breaking rate of the 30-50 mesh (600-300 mu m) petroleum fracturing propping agent is less than 2.58 percent, and the standard of SY/T5108-2014 is less than or equal to 9.0 percent.
The petroleum fracturing propping agent with the granularity of 40-60 meshes (425-250 mu m) is prepared according to the proportion, and the volume density, the apparent density and the breaking degree under different specifications of closing pressure of the petroleum fracturing propping agent are measured according to the SY/T5108-2014 standard, and the result is as follows: bulk density 1.31g/cm3Apparent density 2.75g/cm3(ii) a Under the closing pressure of 40MPa, the breakage rate of the 40-60 mesh (425-250 mu m) petroleum fracturing propping agent is less than 3.01 percent, and the standard of SY/T5108-.
Example 3
The low-density petroleum fracturing propping agent is prepared from the following components:
4 to 6 percent of light-burned bauxite, 6 to 8 percent of bentonite, 0.8 to 1.2 percent of manganese powder, 0.8 to 1.2 percent of light-burned magnesium powder, 0.4 to 0.6 percent of silica fume, 0 to 0.5 percent of over-burned recycled powder and the balance of low-aluminum fly ash.
Wherein, in the light-burned bauxite, Al2O3The mass percentage content of the compound is 70 percent; in the bentonite, the mass percentage of montmorillonite is 85%; in the low-aluminum fly ash, Al2O3Is 36.52 percent by mass, SiO238.56% by mass of Fe2O3The mass percentage of the CaO is 4.05 percent, and the mass percentage of the CaO is 10.35 percent;the light-burned bauxite, the bentonite, the manganese powder, the light-burned magnesium powder, the low-aluminum fly ash and the silica fume are sieved by a 200-mesh sieve, and the passing rate is 99%.
As shown in fig. 1, the preparation method of the low-density petroleum fracturing proppant comprises the following steps:
s1: adding the industrial solid waste low-alumina fly ash crude product which takes quasi-Geer coal as power generation fuel by Inmunogu Datang International tokto power generation Limited company into a straight tube ball mill, removing large materials, and sieving with a 200-300-mesh sieve to obtain low-alumina fly ash ball milled powder;
s2: weighing the following raw materials in percentage by mass: mixing 6.0Kg of light calcined alumina, 8.0Kg of bentonite, 1.0Kg of manganese powder, 1.0Kg of light calcined magnesium powder, 0.50Kg of silica fume, 0.300Kg of overburning recycled powder and 83.2Kg of low-alumina fly ash ball-milled powder obtained in the step S1, homogenizing to obtain mixed powder, mixing the mixed powder with water for pulping, wherein the volume ratio of the mixed powder to the water for pulping is 1:1.5, and obtaining slurry;
s3: grinding the slurry obtained in the step S2 to 600-800 meshes in a ceramic ball mill, wherein the passing rate of the superfine powder slurry after passing through a 600-mesh water sieve is 90-100%, so as to obtain superfine powder slurry, drying the superfine powder slurry in a dryer, then drying 10% of the superfine powder slurry to prepare dry powder with the moisture content of less than or equal to 2.0%, and drying the rest superfine powder slurry to prepare semi-wet powder with the moisture content of 8.0%;
s4: adding water spray to the dry powder and the semi-wet powder obtained in the step S3 in a granulator, granulating and forming, wherein when the dry powder and the semi-wet powder are subjected to water spray granulation and forming in the granulator, the mass percentage of the dry powder is 0-10%, the mass percentage of the semi-wet powder is 90-100%, the addition amount of the dry powder is adjusted according to the rotating speed of the granulator and the water addition amount in the water spray process, the aim is to keep the granulation and forming time at 1.5h to obtain semi-finished product blank balls, the granulation and forming time is 1.5h, the semi-finished product blank balls are dried until the water content is less than 2%, the drying temperature is 105 ℃, then the dried products are classified and screened according to particle size to respectively obtain qualified blank balls, large-particle blank balls and small-particle blank balls, and the qualified blank balls are sieved by a 20-40-mesh standard screen, Sieving the large-particle blank balls by any one of a 30-50-mesh standard sieve and a 40-60-mesh standard sieve to obtain blank balls, wherein the large-particle blank balls are blank balls which cannot be sieved by an upper limit sieve of one of the standard sieves, the small-particle blank balls are blank balls which can be sieved by a lower limit sieve of one of the standard sieves, crushing the large-particle blank balls to 600-800 meshes, mixing the crushed large-particle blank balls with the semi-wet powder in the step S3, and returning the small-particle blank balls to the granulator for re-granulation;
s5, performing temperature programmed sintering on the qualified blank balls obtained in the step S4 in an automatic high-temperature resistance furnace or a rotary kiln, wherein the sintering temperature is 1350 ℃, the sintering heat preservation time is 1.0h, in the step S5, the temperature rising rate of the temperature programmed sintering is 3 ℃/min to 5 ℃/min, the temperature rising rate is 5 ℃/min when the temperature is lower than 1000 ℃, the temperature rising rate is gradually reduced to 3 ℃/min when the temperature rises from 1000 ℃ to 1300 ℃, the time of the temperature programmed sintering is 5.8h to 6.2h, after the sintering is finished, naturally cooling to the normal temperature, and the cooling time is 5h, so that the sintered blank balls are obtained;
s6, screening the fired blank balls obtained in the step S5 step by step, firstly, screening out under-fired blank balls through a color screening machine, wherein the color screening machine marks the colors of the qualified blank balls as red, marks the colors of the qualified blank balls, which are 30% lower than the chroma of the qualified blank balls, as green, the color screening machine screens out the under-fired blank balls marked as green, and returning the obtained under-fired blank balls to the step S5 for re-firing; screening out fired blank balls through the particle size, screening out the fired blank balls through a 20-mesh screen, preliminarily crushing the screened fired blank balls through a jaw crusher before the fired blank balls are subjected to stamping and crushing, stamping and crushing the fired blank balls under 28MPa, vibrating and screening to obtain powder, and crushing the powder into 600-800 meshes through an ultrafine crusher to obtain the fired recycled powder in the step S2; finally, obtaining a finished product blank ball;
and S7, classifying and screening the screened finished product blank balls through a standard screen to obtain the petroleum fracturing propping agent with the mesh number of 20-40 meshes, and obtaining the low-density petroleum fracturing propping agent.
According to the SY/T5108-2014 standard, the volume density, the apparent density and the fracture degree under different specifications of closed pressure of the 20-40-mesh petroleum fracturing propping agent are measured, and the result is as follows: bulk density 1.28g/cm3Apparent density of 2.65g/cm3(ii) a Under the closing pressure of 28MPa, the breaking rate of the 20-40 mesh (850-425 mu m) petroleum fracturing propping agent is less than 0.82%, and the standard of SY/T5108-.
The petroleum fracturing propping agent with the granularity of 30-50 meshes (600-300 mu m) is prepared according to the proportion, and the volume density, the apparent density and the breaking degree under different specifications of closing pressure of the petroleum fracturing propping agent are measured according to the SY/T5108-2014 standard, and the result is as follows: bulk density 1.31g/cm3Apparent density 2.68g/cm3(ii) a Under the closing pressure of 35MPa, the breaking rate of the 30-50 mesh (600-300 mu m) petroleum fracturing propping agent is less than 0.74 percent, and the standard of SY/T5108-2014 is less than or equal to 9.0 percent.
The petroleum fracturing propping agent with the granularity of 40-60 meshes (425-250 mu m) is prepared according to the proportion, and the volume density, the apparent density and the breaking degree under different specifications of closing pressure of the petroleum fracturing propping agent are measured according to the SY/T5108-2014 standard, and the result is as follows: bulk density 1.28g/cm3Apparent density 2.67g/cm3(ii) a Under the closing pressure of 40MPa, the breakage rate of the 40-60 mesh (425-250 mu m) petroleum fracturing propping agent is less than 1.12%, and the standard of SY/T5108-.
Mixing 6.0Kg of light-burned alumina, 8.0Kg of bentonite, 1.0Kg of manganese powder, 1.0Kg of light-burned magnesium powder, 0.50Kg of silica fume, 0.300Kg of over-burned recycled powder and 83.2Kg of low-aluminum fly ash which is an industrial solid waste of Guiger coal serving as power generation fuel, adding water into a ceramic ball mill according to the volume ratio of 1:1.5 to pulp in a ceramic ball mill, drying, granulating, classifying and screening, sintering at 1370 ℃ in an automatic high-temperature resistance furnace, preserving heat for 1h, naturally cooling for 5h to normal temperature, and screening to obtain the petroleum fracturing propping agent with the mesh number of 20-40 meshes (850-425 mu m), 30-50 meshes (600-300 mu m) and 40-60 meshes (425-250 mu m).
Determination of oilVolume density of fracturing propping agent is 1.28g/cm3Apparent density of 2.65g/cm3(ii) a The breaking rate of the 20-40 mesh (850-425 mu m) petroleum fracturing propping agent under the closed pressure of 28Mpa is less than 0.82 percent; the breaking rate of the 30-50 mesh (600-300 mu m) petroleum fracturing propping agent is less than 0.74% under 35Mpa of closing pressure; the breaking rate of the 40-60 mesh (425-250 mu m) petroleum fracturing propping agent is less than 1.12% under the closing pressure of 40 Mpa.
As can be seen from the data of examples 1-3, the low density petroleum fracturing proppant of the present invention has a bulk density of 1.28g/cm3~1.40g/cm3Apparent density of 2.65g/cm3~2.80g/cm3The breaking rate under 28Mpa closing pressure, 35Mpa closing pressure and 40Mpa closing pressure is less than 3%.
The petroleum fracturing propping agent in the prior art, such as a comparison document 1, a fly ash petroleum fracturing propping agent and a preparation method thereof (patent number: 201310148261.3) disclose that the fly ash petroleum fracturing propping agent is prepared from the following components: 1-60% of fly ash; 1 to 30 percent of potassium feldspar powder; the balance of bauxite powder. The volume density of the obtained petroleum fracturing propping agent is 1.50g/cm3~1.60g/cm3Apparent density of 2.55g/cm3~2.70g/cm3And under the closing pressure of 86MPa, the breaking rate is less than or equal to 8 percent.
For example, the comparison document 2 discloses a ceramsite sand petroleum fracturing propping agent and a preparation method thereof (application number: 201710503251.5). the content of fly ash is 40-45%, the content of bauxite is 4-50%, the content of magnesia is 5-10%, the content of quicklime is 2-4%, and the content of bentonite is 1-3%. The apparent density of the obtained ceramsite sand petroleum fracturing propping agent is 2.36-2.42 g/cm 3; the bulk density is 1.39-1.45 g/cm 3; the breaking rate under the condition of 52Mpa is 7-9%.
The volume density of the prior art oil fracturing propping agent such as the above-mentioned comparison documents 1 and 2 is 1.39g/cm3~1.60g/cm3Apparent density of 2.36g/cm3~2.80g/cm3The breaking rate under 28Mpa closing pressure, 35Mpa closing pressure and 40Mpa closing pressure is less than 9%. Compared with the prior art, the low-density petroleum fracturing propping agent has apparent densityUnder the condition of basically not changing, the volume density is reduced by 10% at most compared with the prior art, namely the open gap of the low-density petroleum propping agent is improved, the smoothness of oil and gas products passing through the petroleum fracturing propping agent is increased, then under the same closing pressure, the crushing rates of the low-density petroleum fracturing propping agent of the invention under the closing pressure of 28Mpa, the closing pressure of 35Mpa and the closing pressure of 40Mpa are all lower than the crushing rate of the petroleum fracturing propping agent of the prior art, the proportion of fly ash is increased to 80% when the petroleum fracturing propping agent of the invention is prepared, the proportion of fly ash in comparison documents 1 and 2 is lower than 60%, other auxiliary materials still occupy higher proportion, the proportion of bauxite of the invention is small and can be lower than 10%, even lower than 5%, and the bauxite with large proportion can be used in comparison documents 1 and 2, therefore, the bauxite of natural resources is wasted, and the natural resources are not beneficial to being saved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. The low-density petroleum fracturing propping agent is characterized by being prepared from the following components in percentage by mass:
4 to 6 percent of light-burned bauxite, 6 to 8 percent of bentonite, 0.8 to 1.2 percent of manganese powder, 0.8 to 1.2 percent of light-burned magnesium powder, 0.4 to 0.6 percent of silica fume, 0 to 0.5 percent of over-burned recycled powder and the balance of low-aluminum fly ash; the preparation method of the low-density petroleum fracturing propping agent comprises the following steps:
s1: adding the low-aluminum fly ash crude product into a straight tube ball mill, removing large materials, and sieving with a 200-300-mesh sieve to obtain low-aluminum fly ash ball milled powder;
s2: weighing the following raw materials in percentage by mass: 4 to 6 percent of light-burned bauxite, 6 to 8 percent of bentonite, 0.8 to 1.2 percent of manganese powder, 0.8 to 1.2 percent of light-burned magnesium powder, 0.4 to 0.6 percent of silica fume, 0 to 0.5 percent of over-burned recycled powder from S6 and the balance of the low-aluminum fly ash ball-milled powder obtained in the step S1 are mixed and homogenized to obtain mixed powder, and then the mixed powder is mixed with water for pulping to obtain slurry;
s3: grinding the slurry obtained in the step S2 to 600-800 meshes in a ceramic ball mill to obtain superfine powder slurry, drying the superfine powder slurry in a dryer, drying 5-15 wt% of the superfine powder slurry to obtain dry powder with the moisture content of less than or equal to 2.0%, and drying the rest superfine powder slurry to obtain semi-wet powder with the moisture content of 7.5-8.5%;
s4: adding water to spray the dry powder and the semi-wet powder obtained in the step S3 in a granulator, granulating and forming to obtain semi-finished blank balls, wherein the granulation and forming time is 1.4-1.6 h, drying the semi-finished blank balls, classifying and screening according to particle size to respectively obtain qualified blank balls, large-particle blank balls and small-particle blank balls, crushing the large-particle blank balls to 600-800 meshes, mixing with the semi-wet powder obtained in the step S3, and returning the small-particle blank balls to the granulator for re-granulation;
s5, heating and sintering the qualified blank balls obtained in the step S4 in an automatic high-temperature resistance furnace or a rotary kiln by a program, wherein the sintering temperature is 1350 +/-20 ℃, the sintering heat preservation time is 0.8-1.2 h, and after the sintering is finished, naturally cooling to the normal temperature for 5h to obtain the sintered blank balls;
s6, screening the fired blank balls obtained in the step S5 step by step, firstly screening out under-fired blank balls through a color screening machine, then screening out over-fired blank balls through particle size, finally obtaining finished product blank balls, returning the under-fired blank balls to the step S5 for re-firing, punching and crushing the over-fired blank balls under 27-29 MPa, then vibrating and screening to obtain powder, and crushing the powder into 600-800 meshes through an ultrafine grinder as the over-fired recycled powder in the step S2;
and S7, grading and screening the screened finished product blank balls through a standard screen to obtain the low-density petroleum fracturing propping agent.
2. The low density oil fracturing proppant of claim 1, whereinIn the light-burned bauxite, Al2O3The mass percentage content of the compound is 70-75 percent; in the bentonite, the mass percentage of the montmorillonite is 85-90%; in the low-aluminum fly ash, Al2O333.08 to 50.10 percent of SiO235.10 to 42.67 percent of Fe2O3The mass percentage of the CaO is 1.8-4.0%, and the mass percentage of the CaO is 8-12%; the light-burned bauxite, the bentonite, the manganese powder, the light-burned magnesium powder, the low-aluminum fly ash and the silica fume are sieved by a 200-mesh sieve.
3. The low-density oil fracturing propping agent of claim 1, wherein in step S2, the volume ratio of the mixed powder and the water mixed slurry is 1: 1.5.
4. The low-density oil fracturing propping agent of claim 1, wherein in step S3, the passing rate of the ultra-fine powder slurry after passing through a 600-mesh water screen is 90% -100%.
5. The low-density oil fracturing propping agent of claim 1, wherein in step S4, when the dry powder and the semi-wet powder are subjected to water spray granulation and molding in the granulator, the mass percentage of the dry powder is 0-10%, and the mass percentage of the semi-wet powder is 90-100%.
6. The low-density petroleum fracturing proppant of claim 1, wherein in step S4, the qualified green pellets are green pellets screened through any one of standard sieves in the range of 20-40 mesh standard sieves, 30-50 mesh standard sieves and 40-60 mesh standard sieves, the large-particle green pellets are green pellets that cannot be screened through the upper limit of one of the standard sieves, and the small-particle green pellets are green pellets that can be screened through the lower limit of one of the standard sieves.
7. The low density petroleum fracturing proppant of claim 1, wherein in step S4, the semi-finished green pellets are dried to a moisture content of less than 2% and a drying temperature of 103 ℃ to 107 ℃.
8. The low-density oil fracturing proppant of claim 1, wherein in step S5, the temperature-programmed rate is 3 ℃/min to 5 ℃/min, and the temperature-programmed time is 5.8h to 6.2 h.
9. The low-density oil fracturing propping agent of claim 1, wherein in step S6, said color screening machine marks the color of said qualified green balls as red, marks the color of said qualified green balls as green, said color screening machine screens out said green marked green as said under-fired green balls, said over-fired green balls are screened out by a 20-mesh screen, and said over-fired green balls obtained after screening are preliminarily crushed by a jaw crusher before being crushed by said punching.
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