CN103172354A - Preparation method of fracturing propping agent for exploiting shale gas - Google Patents
Preparation method of fracturing propping agent for exploiting shale gas Download PDFInfo
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Abstract
The invention discloses a preparation method of a fracturing propping agent for exploiting shale gas. The method comprises the following steps of: with low-grade alum earth as the main raw material, adding a composite sintering aid on the basis of the main raw material; and forming mixed sludge by taking a stainless steel ball as a grinding medium and using a continuous dry grinding process and a continuous wet grinding process, then, aging and carrying out spray granulation to obtain loose granules, dispersing the granules, then, rolling by using a ball forming mill to obtain a semi-finished product of a blank ball, drying the semi-finished product of the blank ball, and then, sintering the semi-finished product of the blank ball in a high-temperature mechanical shaft kiln or rotary kiln to obtain the special ultralow-density and high-strength fracturing propping agent for exploiting shale gas. The continuous dry grinding process and the continuous wet grinding process are adopted in the method, and the high-mass steel ball is used as the grinding medium, so that the uniformity and the stability of all raw materials in the slurry are ensured, the ball milling efficiency is increased, and no grinding aid is required. The formation of a long columnar mullite is promoted through a sintering way integrated with the continuous dry grinding process, the continuous wet grinding process, the composite sintering aid and the mechanical shaft kiln or rotary kiln, and the content of the columnar mullite in the product is up to 70-80%.
Description
Technical field
The present invention relates to a kind of shale gas exploitation with the preparation method of fracturing propping agents, belong to new material technology field.
Background technology
Shale gas and conventional reservoir gas are hidden different, and shale is the source rock that Sweet natural gas generates, and are also reservoir and the cap rocks of assembling and preserve Sweet natural gas.The reservoir of shale gas reservoir generally is the physical property characteristic of low hole, low permeability, and the resistance ratios conventional gas of air-flow is large.China's shale gas porosity is generally 1% to 3%, and the shale gas permeability of reservoir is low, and the exploitation difficulty is larger, so the ultimate recovery factor of shale gas depends on effective fracturing methods.
In fracturing technology, fracturing liquid is produced the crack to the stratum, for passage is opened in the migration of shale gas, for preventing under the formation closure pressure condition, the crack is slowly closed, stop the shale gas migration, need to use fracturing propping agents, fracturing propping agents enter the stratum with fracturing liquid, rest in slit after fracturing liquid is made seam, stop crack closure, form the support belt of a high flow conductivity, the assurance shale gas is successfully migrated.Therefore, fracturing propping agents be affect fracturing technology to the pass factor.Because propping agent need to rest on the underground of several kms, and formation closure pressure is large, and fracturing propping agents need that not only good temperature tolerance is arranged, and also enough anti-pressure abilities will be arranged.
At present widely used propping agent has natural siliceous sand, the low-density aluminum silicate proppants of medium tenacity, the artificial highdensity aluminum oxide of medium tenacity and natural sand or the artificial stays agent of silicate propping agent, high-intensity bauxitic clay and high-intensity zirconium silicate propping agent and coating Procuring coating and curable coating resin on frscturing market.
The existing patent report of development for preparing the oil fracturing ceramsite propping agent with raw mineral materialss such as bauxitic clays.Be that 201010231375.0 Chinese patent discloses a kind of high-strength ceramic proppant as application number, its raw material consists of: bauxitic clay raw material 80～90%, barite 2～10%, alum 0.1～0.6%, ferric oxide 4～10%, manganese ore stone flour 3～8%; Application number is that 201210274744.3 Chinese patent discloses a kind of low density petroleum fracturing propping agent, calculates by weight, comprises 40～90 parts of bauxitic clays, 1～30 part of 5～30 parts of clays and supplementary additive.It is main raw material that aforementioned ceramsite propping agent all adopts the fine aluminum alumina, because high-quality resource is day by day deficient, saves again cost simultaneously for avoiding the wasting of resources, and preparing ceramsite propping agent with the alternative fine aluminum alumina of low-grade bauxite becomes inexorable trend.Application number is that 201210326914.8 Chinese patent discloses the low-grade bauxite ore deposit and prepares ceramsite propping agent, it is prepared from by the raw material of following mass percent: bauxite 85-94%, clay 0-5%, iron oxide 2-6%, titanium dioxide 0-4%, Manganse Dioxide 2-6%, pass through ball milling, moulding, burn till and make product.This invention has reduced the requirement of ceramsite sand propping agent to bauxite grade, reduced the raw materials cost of product, but a large amount of fusing point low and high temperature volatile matter has been introduced in this invention, cannot effectively control the propping agent crystalline structure, and the fluctuation of bauxitic clay raw materials quality causes the propping agent performance to fluctuate thereupon.Patent CN201210116790.0 discloses a kind of production technique of utilizing low-grade bauxite to prepare ceramsite propping agent, and the main body process comprises: will be made into compound with auxiliary material after low-grade bauxite ore reduction; Secondary wet-milling to mud granularity is 5～20 microns, the mud after old is pumped into spray-drying tower carry out breaing up after drying-granulating forms discrete particle, sends into after the rolling granulation of further spraying to dry-burn till in system ensemble and dries, burns till; The waste heat that produces in sintering process leads to the spray-drying tower utilization.This invention has adopted the low-grade bauxite ore deposit as major ingredient, played active effect to making rational use of resources, reduce energy consumption, but there is following limitation in the method: (1) adopts at least 24 intermittent ball mills (specifically seeing Fig. 1) in especially wet-milling step in actual production process, need a large amount of equipment and manpower, maintenance cost is high, and the investment floor space is large.Simultaneously because the slurry gap of every table grinder ball milling is larger, needs further homogenizing, thereby affected production schedule, and Production Flow Chart is difficult to control, the large and quality product of production cost easily fluctuates; (2) adopt the mode of intermittent ball milling, can not serialization production; (3) adopting alumina balls during ball milling is grinding medium, and because the alumina balls quality is light, Ball-milling Time is long, and efficient is low, and energy consumption is large, and needs the interpolation grinding aid; The crystal formation of the propping agent of (4) producing is the special granular mullite alternate with column, and wherein the ratio of rod-like mullite only accounts for 40-50%, and due to the existence of a large amount of granular mullites, the product performance mechanical property is not good.
Summary of the invention
For the deficiency of above-mentioned technology, the invention provides the preparation method that fracturing propping agents are used in a kind of shale gas exploitation.The method is added the complex sintering aids of Li-Mg contained system on silicon take low-grade bauxite as main raw material on the basis of major ingredient; Take Stainless Steel Ball as grinding medium, first adopt continous way dry method ball-milling technology, then continuous wet-grinding, form mixing mud, then carry out oldly, mist projection granulating obtains discrete particle; It is the powder of 5～20 microns that the powder particle is broken up as grain graininess, obtain work in-process base ball through the nodulizer rolling, burn till at high-temperature machinery shaft kiln or rotary kiln after oven dry, by controlling firing process, with lower production cost, prepare the special-purpose fracturing propping agents of extremely-low density high strength shale gas efficiently.
Technical scheme of the present invention is: a kind of shale gas exploitation preparation method of fracturing propping agents is characterized in that:
(1) raw material and weight part (require the granularity of all raw materials all＜10mm):
Major ingredient: 80～95 parts of low-grade bauxites, 2～12 parts of kaolin; Complex sintering aids: 0.5～1 part, talcum, 0.2～0.5 part of diopside, 0.2～0.8 part of triphane, 0.1～1 part of illite, 0.2～1 part of silicon powder;
The chemical constitution of described low-grade bauxite and mass percent are Al
2O
344-55%, SiO
240-52%, TiO
21-2%, K
2O0.1-0.17%, Na
2O0.05-0.12%, CaO≤0.8%, MgO≤0.2%;
(2) continuously dry grinding: the raw material that step (1) is prepared is crossed 180 mesh sieves by the automatical feeding system continous way dry method ball mill ball milling of packing into, obtains expecting powder; Milling parameters is: take Stainless Steel Ball as grinding medium, material is 1:2～3 with the mass ratio of ball; Homogenizing in automatic cylindrical shell, the long 7.48m of ball mill barrel, barrel diameter 1.5m;
(3) continuous wet-grinding: step (2) gained powder is sent into the continuous wet-grinding machine by automatical feeding system carry out continuous wet-grinding to mud granularity and reach 5～20 microns, then send into the old 24 ± 2h of suction pit; Milling parameters is: take Stainless Steel Ball as grinding medium, the mass ratio of material, ball, water is 1:2.5～3.5:0.5; Homogenizing in automatic cylindrical shell, the long 7.2m of ball mill barrel, barrel diameter 1.3m;
(4) mist projection granulating: the mud after step (3) is old pumps into spray-drying tower and carries out drying-granulating, obtains water content and be 0.1～0.5% discrete particle;
(5) powder material scattering: use the equipment of breaing up that the discrete particle of step (4) gained is broken up powder as particle diameter after continuous wet-grinding again;
(6) step (5) gained powder being obtained granularity through the nodulizer rolling is the spherical base substrate of 20-40 purpose propping agent;
(7) with the spherical base substrate of the resulting propping agent of step (6) dry 24 ± 2h at 100～150 ℃ of temperature, then
A, be warming up to 1200～1350 ℃ with the rate of heating of 8～25 ℃/min from room temperature burn till in cement mechanized shaft kiln, insulation 2～6h, insulation 1h 800 ℃ time the wherein, insulation 1h in the time of 1000 ℃; With the speed of cooling cooling of 25～45 ℃/min, obtain the special-purpose fracturing propping agents product of the high-intensity shale gas of extremely-low density again.
B, fire in rotary kiln and obtain the special-purpose fracturing propping agents product of the high-intensity shale gas of extremely-low density; The rotating speed of described rotary kiln is 1.5-2 rev/min, and the highest firing temperature is 1380-1420 ℃, long 28 meters of kiln, and the kiln out temperature is respectively 350,850 ℃, 1.5 hours ball base residence time.
Wherein, preferably adopt in cement mechanized shaft kiln and burn till.
The present invention adopts continous way dry method humidification method ball-milling technology, and this kind ball-milling technology adopts equipment few, and floor space is few, has reduced cost of investment; The simple (see figure 2) of flow process can serialization production.
Wherein: the intermittent ball mill contrast of continous way dry method ball mill of the present invention and continous way wet method ball mill mode and Fig. 1 is as follows:
Load contrast: according to same fineness requirement and grinding medium, per hour 3 tons of dischargings of continuous type ball mill, 2 tons of the intermittent ball mill of 2 tons dischargings in every 12 hours.2 are ground (namely dry grinding continuously and 1 continuous wet-grinding for 1) 18 discharging output of intermittent ball mill that load equaled 2 tons in 1 day continuously, and wherein the intermittent ball mill charging did not count with the time of discharging.
The power contrast: the power that continuous type ball mill (dry grinding and wet-milling) goes out 1 ton of material is 250*0.8*1/3*2=133KW; The power that the intermittent ball mill of 2 tons goes out 1 ton of material is 50*0.8*6=240KW.
Grinding medium of the present invention is Stainless Steel Ball, and it has high specific gravity, low abrasion, high sphericity and desirable hardness, can guarantee grinding efficiency and product performance.Draw through a large amount of experimental datas: Stainless Steel Ball ratio aluminum oxide mill ball milling time under condition of equivalent can shorten more than 1.5 times, and in the life-time service process, repeatedly abrasion and the subsurface defect of Stainless Steel Ball are smaller, can guarantee for a long time high grinding efficiency.
The present invention adopts cement mechanized shaft kiln to fire and forms, whole process adopts mechanized operation, wholly computer controlled, guarantee production efficiency, reduce labour intensity, less manufacturing cost, can avoid crystal to divide phase reaction in the insulation simultaneously for a long time of multiple spot under the condition of high temperature simultaneously, can not form the difficult problem of long column shape mullite phase, avoid internal stress to produce, the quality of enhancing product performance.
The special-purpose fracturing propping agents performance index of shale gas of the present invention are according to SY/T5108-2006, and " fracturing propping agents performance test recommend method " tested, and test result is: volume density≤1.45g/cm
3Volume density≤2.65g/cm
352MPa locking pressure percentage of damage 1.5～3%; 69MPa locking pressure percentage of damage 5～7%; Acid resistance＜3%.
The inventive method compared with prior art has following significant advantage:
1, the present invention dry grinds by continous way and improves the material homogeneity, promotes solid state sintering by complex sintering aids with the continuous type wet grinding process; Jointly promote the formation of long column shape mullite at the firing mode of mechanical type shaft kiln or the insulation of rotary kiln different sites by controlling the ball base, in product, the content of rod-like mullite reaches 70-80%.
2, the present invention adopts continous way dry method ball milling to add wet-grinding technology and relative device, guarantees homogeneity, the stability of each raw material in slurry, has improved grinding efficiency, and employing equipment is few, and floor space is few, has reduced cost of investment, simultaneously all right serialization production, and energy consumption is little; Adopting simultaneously the large Stainless Steel Ball of quality is grinding medium, improves mill efficiency.
3, special-purpose fracturing propping agents of shale gas of the present invention and preparation method thereof utilize ready-made ripe device fabrication, need not to increase other equipment investments, can produce the special-purpose fracturing propping agents of high-performance shale gas with lower cost, have significant social benefit, environmental benefit, economic benefit.
Description of drawings
Fig. 1 is the process flow sheet of intermittent type ball milling method;
Fig. 2 is the process flow sheet of continous way dry grinding+continous way of the present invention wet-milling.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but be not limited only to this.
Embodiment 1:
The raw material index: the chemical composition of low-grade bauxite and mass percent are: Al
2O
344%, SiO
250%, TiO
21.2%, K
2O+Na
2O0.18%, CaO0.6%, MgO0.15%.The lithium amount that contains of triphane is 3.8wt%.The performance index of other raw materials see Table 1.
The chemical constitution of other raw materials of table 1 and weight part
(1) obtain respectively satisfactory each raw material accurate proportioning by weight, low-grade bauxite: kaolin: talcum: diopside: triphane: illite: silicon powder=86 part: 11 parts: 1 part: 0.5 part: 0.5 part: 0.5 part: 0.5 part.
(2) raw material that step 1 is prepared is crossed 180 mesh sieves by the automatical feeding system continous way dry method ball mill ball milling of packing into, obtains the formulation material powder.Milling parameters is: the long 7.48m of ball mill barrel, and barrel diameter 1.5m, material: the ball mass ratio is 1:2.5, and per hour discharging is 3.3 tons,
(3) continuous wet-grinding: step (2) gained powder is sent into the continuous wet-grinding machine by automatical feeding system carry out continuous wet-grinding to mud granularity and reach 20 microns, then send into the old 24h of suction pit; Milling parameters is: take Stainless Steel Ball as grinding medium, the mass ratio of material, ball, water is 1:2.5:0.5, the long 7.2m of ball mill barrel, barrel diameter 1.3m;
(4) mist projection granulating: the mud after step (3) is old pumps into spray-drying tower and carries out drying-granulating, obtains water content and be 0.1% discrete particle;
(5) powder material scattering: use the equipment of breaing up that the resulting discrete particle of step (4) is broken up powder as particle diameter after wet-milling again;
(6) step (5) gained powder being obtained granularity through the nodulizer rolling is the spherical base substrate of 20-40 purpose propping agent;
(7) with the spherical base substrate of the resulting propping agent of step (6) after dry 24h at 100～150 ℃ of temperature, being warming up to 1200～1350 ℃ with the rate of heating of 8～25 ℃/min from room temperature in cement mechanized shaft kiln burns till, insulation 2～6h, 800 ℃ of time insulation 1h wherein, insulation 1h in the time of 1000 ℃, with the cooling of 25～45 ℃/min speed of cooling, obtain the special-purpose fracturing propping agents product of the high-intensity shale gas of extremely-low density again.
According to oil and gas industry standard " fracturing propping agents performance test recommend method " SY/T5108-2006, the ceramsite propping agent of the present embodiment preparation is tested, main performance index see Table 2.
Embodiment 2:
The raw material index: the chemical composition of low-grade bauxite and mass percent are: Al
2O
345%, SiO
249%, TiO
21.5%, K
2O+Na
2O0.18%, CaO0.5%, MgO0.18%.The other the same as in Example 1.
(1) obtain respectively satisfactory each raw material accurate proportioning by weight: low-grade bauxite: kaolin: talcum: diopside: triphane: illite: silicon powder=87 part: 10 parts: 0.8 part: 0.5 part: 0.7 part: 0.3 part: 0.7 part.
(2) raw material that step (1) is prepared is crossed 180 mesh sieves by the automatical feeding system continous way dry method ball mill ball milling of packing into, obtains the formulation material powder.Milling parameters is: the long 7.48m of ball mill barrel, and barrel diameter 1.5m, material: ball=1:2.8, per hour discharging is 3.2 tons.
(3) continuous wet-grinding: step (2) gained powder is sent into the continuous wet-grinding machine by automatical feeding system carry out continuous wet-grinding to mud granularity and reach 15 microns, then send into the old 26h of suction pit; Milling parameters is: take Stainless Steel Ball as grinding medium, the mass ratio of material, ball, water is 1:2.8:0.5, the long 7.2m of ball mill barrel, barrel diameter 1.3m;
(4) mist projection granulating: the mud after step (3) is old pumps into spray-drying tower and carries out drying-granulating, obtains water content and be 0.3% discrete particle;
(5) powder material scattering: use the equipment of breaing up that the discrete particle of step (4) gained is broken up powder as particle diameter after wet-milling again;
(6) step (5) gained powder being obtained granularity through the nodulizer rolling is the spherical base substrate of 20-40 purpose propping agent;
(7) with the spherical base substrate of the resulting propping agent of step (6) after dry 26h at 100～150 ℃ of temperature, fire in rotary kiln and obtain the special-purpose fracturing propping agents product of the high-intensity shale gas of extremely-low density; The rotating speed of described rotary kiln is 1.5 rev/mins, and the highest firing temperature is 1380-1420 ℃, long 28 meters of kiln, and the kiln out temperature is respectively 350,850 ℃, 1.5 hours ball base residence time.
According to oil and gas industry standard " fracturing propping agents performance test recommend method " SY/T5108-2006, the ceramsite propping agent of the present embodiment preparation is tested, main performance index see Table 2.
Embodiment 3:
The raw material index: the chemical composition of low-grade bauxite and mass percent are: Al
2O
344.5%, SiO
248%, TiO
21.1%, K
2O+Na
2O0.2%, CaO0.8%, MgO0.2%.The performance index of other raw materials see Table 1.
(1) obtain respectively satisfactory each raw material accurate proportioning by weight: low-grade bauxite: kaolin: talcum: diopside: triphane: illite: silicon powder=86.5 part: 11 parts: 1 part: 0.3 part: 0.5 part: 0.5 part: 0.2 part.
(2) raw material that step (1) is prepared is crossed 180 mesh sieves by the automatical feeding system continous way dry method ball mill ball milling of packing into, obtains the formulation material powder, milling parameters is: the long 7.48m of ball mill barrel, barrel diameter 1.5m, material: ball=1:3, per hour discharging is 3.5 tons.
(3) continuous wet-grinding: step (2) gained powder is sent into the continuous wet-grinding machine by automatical feeding system carry out continuous wet-grinding to mud granularity and reach 8 microns, then send into the old 22h of suction pit; Milling parameters is: take Stainless Steel Ball as grinding medium, the mass ratio of material, ball, water is 1:3.5:0.5, the long 7.2m of ball mill barrel, barrel diameter 1.3m;
(4) mist projection granulating: the mud after step (3) is old pumps into spray-drying tower and carries out drying-granulating, obtains water content and be 0.5% discrete particle;
(5) powder material scattering: use the equipment of breaing up that the discrete particle of step (4) gained is broken up powder as particle diameter after wet-milling again;
(6) step (5) gained powder being obtained granularity through the nodulizer rolling is the spherical base substrate of 20-40 purpose propping agent;
(7) with the spherical base substrate of the resulting propping agent of step (6) after dry 22h at 100～150 ℃ of temperature, being warming up to 1200～1350 ℃ with the rate of heating of 8～25 ℃/min from room temperature in cement mechanized shaft kiln burns till, insulation 2～6h, 800 ℃ of time insulation 1h wherein, insulation 1h in the time of 1000 ℃, with the cooling of 25～45 ℃/min speed of cooling, obtain the special-purpose fracturing propping agents product of the high-intensity shale gas of extremely-low density again.
According to oil and gas industry standard " fracturing propping agents performance test recommend method " SY/T5108-2006 to the present embodiment
The ceramsite propping agent of preparation is tested, and main performance index see Table 2.
The performance index of the ceramsite propping agent of table 2 embodiment 1-3 preparation
Claims (6)
1. the preparation method of shale gas exploitation use fracturing propping agents, is characterized in that,
(1) raw material and weight part:
Major ingredient: 80～95 parts of low-grade bauxites, 2～12 parts of kaolin;
Complex sintering aids: 0.5～1 part, talcum, 0.2～0.5 part of diopside, 0.2～0.8 part of triphane, 0.1～1 part of illite, 0.2～1 part of silicon powder;
The chemical constitution of described low-grade bauxite and mass percent are Al
2O
344-55%, SiO
240-52%, TiO
21-2%, K
2O0.1-0.17%, Na
2O0.05-0.12%, CaO≤0.8%, MgO≤0.2%;
(2) continuously dry grinding: the raw material that step (1) is prepared is crossed 180 mesh sieves by the automatical feeding system continuous dry method ball mill ball milling of packing into, obtains expecting powder; Milling parameters is: take Stainless Steel Ball as grinding medium, the mass ratio of raw material and Stainless Steel Ball is 1:2～3;
(3) continuous wet-grinding: step (2) gained powder is sent into the continuous wet-grinding machine by automatical feeding system carry out continuous wet-grinding to mud granularity and reach 5～20 microns, then send into the old 24 ± 2h of suction pit; Milling parameters is: take Stainless Steel Ball as grinding medium, the mass ratio of raw material, Stainless Steel Ball and water is 1:2.5～3.5:0.5;
(4) mist projection granulating: the mud after step (3) is old pumps into spray-drying tower and carries out drying-granulating, obtains water content and be 0.1～0.5% discrete particle;
(5) powder material scattering: use the equipment of breaing up that the discrete particle of step (4) gained is broken up powder as particle diameter after continuous wet-grinding again;
(6) step (5) gained powder being obtained granularity through the nodulizer rolling is the spherical base substrate of 20-40 purpose propping agent;
(7) with the spherical base substrate of the resulting propping agent of step (6) dry 24 ± 2h at 100～150 ℃ of temperature, then fire in cement mechanized shaft kiln or rotary kiln and obtain the special-purpose fracturing propping agents of the high-intensity shale gas of extremely-low density.
2. a kind of shale gas exploitation as claimed in claim 1 with the preparation method of fracturing propping agents, is characterized in that, described step (7) is fired in cement mechanized shaft kiln and obtained the special-purpose fracturing propping agents of the high-intensity shale gas of extremely-low density; Be warming up to 1200～1350 ℃ with the rate of heating of 8～25 ℃/min from room temperature and burn till in cement mechanized shaft kiln, insulation 2～6h, insulation 1h 800 ℃ time the wherein, insulation 1h in the time of 1000 ℃; Lower the temperature with the speed of cooling of 25～45 ℃/min again.
3. a kind of shale gas exploitation as claimed in claim 1 with the preparation method of fracturing propping agents, is characterized in that, described step (7) is fired in rotary kiln and obtained the special-purpose fracturing propping agents of the high-intensity shale gas of extremely-low density; The rotating speed of described rotary kiln is 1.5-2 rev/min, and the highest firing temperature is 1380-1420 ℃.
4. a kind of shale gas exploitation as claimed in claim 3 with the preparation method of fracturing propping agents, is characterized in that, long 28 meters of described rotary kiln, and the kiln out temperature is respectively 350,850 ℃, 1.5 hours ball base residence time.
5. a kind of shale gas exploitation as described in any one in claim 1-4 with the preparation method of fracturing propping agents, is characterized in that, described step (2) is dry grinded continuously with homogenizing in the automatic cylindrical shell of ball mill, the long 7.48m of cylindrical shell, barrel diameter 1.5m.
6. a kind of shale gas exploitation as described in any one in claim 1-4 with the preparation method of fracturing propping agents, is characterized in that, described step (3) continuous wet-grinding is with homogenizing in the automatic cylindrical shell of ball mill, the long 7.2m of cylindrical shell, barrel diameter 1.3m.
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| CN104130764A (en) * | 2013-08-07 | 2014-11-05 | 郑州市润宝耐火材料有限公司 | Additive for fracturing propping agent, fracturing propping agent and preparation method |
| CN104150882A (en) * | 2014-06-30 | 2014-11-19 | 金刚新材料股份有限公司 | Preparation method of aluminum oxide microbeads |
| CN105524607A (en) * | 2016-01-12 | 2016-04-27 | 金刚新材料股份有限公司 | Method for preparing low-density ceramsite proppant from high-alumina fly ash |
| CN105586027A (en) * | 2016-03-17 | 2016-05-18 | 成都创源油气技术开发有限公司 | Preparation method of shale gas production fracturing propping agent |
| CN111960807A (en) * | 2020-08-24 | 2020-11-20 | 垣曲县刚玉陶粒有限责任公司 | Preparation method of medium-density ultrahigh-strength ceramsite proppant |
| CN112500170A (en) * | 2020-12-21 | 2021-03-16 | 西南石油大学 | Low-density silicon carbide-based complex-phase ceramsite proppant and preparation method thereof |
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| CN104130764B (en) * | 2013-08-07 | 2017-02-08 | 郑州市润宝耐火材料有限公司 | Additive for fracturing propping agent, fracturing propping agent and preparation method |
| CN104150882A (en) * | 2014-06-30 | 2014-11-19 | 金刚新材料股份有限公司 | Preparation method of aluminum oxide microbeads |
| CN104150882B (en) * | 2014-06-30 | 2015-12-02 | 金刚新材料股份有限公司 | A kind of aluminum oxide preparation of microbeads |
| CN105524607A (en) * | 2016-01-12 | 2016-04-27 | 金刚新材料股份有限公司 | Method for preparing low-density ceramsite proppant from high-alumina fly ash |
| CN105524607B (en) * | 2016-01-12 | 2018-01-26 | 金刚新材料股份有限公司 | A kind of method that low-density ceramic proppant is prepared using aluminous fly-ash as raw material |
| CN105586027A (en) * | 2016-03-17 | 2016-05-18 | 成都创源油气技术开发有限公司 | Preparation method of shale gas production fracturing propping agent |
| CN111960807A (en) * | 2020-08-24 | 2020-11-20 | 垣曲县刚玉陶粒有限责任公司 | Preparation method of medium-density ultrahigh-strength ceramsite proppant |
| CN112500170A (en) * | 2020-12-21 | 2021-03-16 | 西南石油大学 | Low-density silicon carbide-based complex-phase ceramsite proppant and preparation method thereof |
| CN112500170B (en) * | 2020-12-21 | 2021-11-30 | 西南石油大学 | Low-density silicon carbide-based complex-phase ceramsite proppant and preparation method thereof |
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