CN106396624B - A kind of gangue proppant and preparation method thereof - Google Patents

A kind of gangue proppant and preparation method thereof Download PDF

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CN106396624B
CN106396624B CN201610784110.0A CN201610784110A CN106396624B CN 106396624 B CN106396624 B CN 106396624B CN 201610784110 A CN201610784110 A CN 201610784110A CN 106396624 B CN106396624 B CN 106396624B
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gangue
proppant
content
powder
ball
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CN106396624A (en
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刘广峰
吴云海
甄远
黄兆丰
邓超
陈旭东
曹晓伟
张旭
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Beijing Poly-Doctor Petroleum Technology Co., Ltd.
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BEIJING POLY-DOCTOR PETROLEUM TECHNOLOGY Co Ltd
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Abstract

A kind of gangue proppant and preparation method thereof, the gangue are the solid waste discharged during coal mining process and coal washing.Proppant of the invention can either efficiently use solid waste gangue, it is gangue again using providing new approach, it can be conducive to improve the intensity of firing haydite again, to adapt to the support of the high deep-seated oil gas well pressure-break of clossing pressure, it is characterized in that, the proppant is ceramic particle, and the ceramic particle is formed by coal gangue ceramic is pug fired, and the Coal gangue pottery porcelain pug refers in the raw material components of ceramic material using gangue roasting powder as major ingredient.

Description

A kind of gangue proppant and preparation method thereof
Technical field
The present invention relates to well fracturing seam support technology, especially a kind of gangue proppant and preparation method thereof, The gangue is the solid waste of discharge during coal mining process and coal washing.Proppant of the invention can either efficiently use solid Body waste gangue is gangue again using providing new approach, and can be conducive to improve the intensity of firing haydite, To adapt to the support of the high deep-seated oil gas well pressure-break of clossing pressure.
Background technique
When petroleum gas deep mining, high clossing pressure deposits of low permeability makes Oil gas-containing rock layer after frac treatment It splits, oil gas collects from the channel of cracking initiation.Enter Filling in company with high-pressure solution with haydite backing material to exist In rock crack, playing the role of support crack, stress is not discharged and is closed, to keep high flow conductivity, keeps oil gas smooth It is logical, increase yield.Therefore, in recent decades, to develop deep-seated oil, gas well, its yield is improved, fracturing technology is widely adopted. Since Selid propping agent closely related therewith is the key that one of this technique application quality, for this purpose, scientific research people both domestic and external Member has put into numerous studies to the manufacturing method of high-quality Selid propping agent.Existing support agent producing process includes sintering process and electricity Molten two kinds of blowing process.More ground manufacturers mostly use electric smelting blowing process at home, and the product of production is mostly Medium and low intensity, and power consumption It is relatively high.The Selid propping agent and its manufacturing method for the CN1046776A that Chinese invention patent bulletin is delivered just belong to electric smelting blowing Method.Foreign countries are more using sintering process, but to make to produce serialization, automation, crucial balling-up process uses fluidized bed mud Starch blowing process or disc type method.The manufacture sintered bauxite ball technique of British patent GB2079261A, be will containing bauxite and Then the aqueous suspension material of bonding agent is sintered by fluidization blowing process pelletizing.The technique serialization, the degree of automation Height, but invest greatly, be not suitable for current China's national situation, product quality is also relatively good, but expensive, generally domestic similar product 6~8 times.For both at home and abroad in such a way that bauxite prepares Selid propping agent as major ingredient, inventors believe that, it should to its into Row changes, and especially efficiently uses solid waste in a manner of turning waste into wealth, and with raw material cheap, simple process, it is energy-efficient, Product is of fine quality to open up new process flow and process conditions for target on well fracturing proppant.For this purpose, the present inventor is complete At the present invention, a kind of simple process is provided, efficient, energy conservation, good product quality, at low cost, the gangue of suitable China's national situation Proppant in high intensity and preparation method thereof, to support widely used deep-seated oil gas well Fracturing Technology.
Summary of the invention
The present invention is in view of the deficiencies in the prior art or insufficient, provides a kind of gangue proppant and its preparation side Method, the gangue are the solid waste of discharge during coal mining process and coal washing.Proppant of the invention can either be effectively sharp It is gangue again using providing new approach, and can be conducive to improve firing haydite with solid waste gangue Intensity, to adapt to the support of the high deep-seated oil gas well pressure-break of clossing pressure.
Technical scheme is as follows:
A kind of gangue proppant, which is characterized in that the proppant is ceramic particle, and the ceramic particle is by gangue Ceramic material is fired, and the Coal gangue pottery porcelain pug refers in the raw material components of ceramic material is with gangue roasting powder Major ingredient.
The gangue roasting powder content is 80wt%~95wt%.
It include auxiliary material in the raw material components of the ceramic material, the auxiliary material includes clay and many oxide.
The many oxide is Fe2O3, MgO and MnO2；The clay is mild-clay.
Fe2O3Feedstock Component content is 1wt%~15wt%, and MgO Feedstock Component content is 0.5wt%~10wt%, MnO2 Feedstock Component content is 0.5wt%~10wt%, and raw clay constituent content is 1wt%~10wt%.
The main chemical compositions and its weight content of the gangue roasting powder are as follows: Al2O355~70%, SiO2 15~30%, Fe2O32~10.5%, TiO22~5.5%.
The gangue proppant is with α-Al2O3(corundum) structure is principal crystalline phase, and multi-component oxide and mild-clay are total Molten rear and α-Al2O3Form the combination of solid solution and glass phase, product quality indicator are as follows: percentage of damage < 2~4%；Circularity, ball Degree is >=0.9；Volume density≤1.65g/cm3；Apparent density≤2.75g/cm3；Turbidity≤10FTU；During surface smoothness is；Acid is molten Xie Du≤4.5%；Flow conductivity >=22.27 μm2·cm。
A kind of preparation method of gangue proppant, which is characterized in that including gangue roasting, crush, total mill, mixed grind system Ceramic material is obtained, loosened, balling-up, screening for the first time, firing, polished and sieve for the second time；The raw material group of the ceramic material Divide and content is as follows: it is 80wt%~95wt%, Fe that gangue, which roasts powder content,2O3Feedstock Component content be 1wt%~ 15wt%, MgO Feedstock Component content are 0.5wt%~10wt%, MnO2Feedstock Component content is 0.5wt%~10wt%, is glued Native Feedstock Component content is 1wt%~10wt%.
The temperature of the gangue roasting is 1000 DEG C~1340 DEG C；Described crush is multi-stage crushing, the multi-stage crushing For three-level crushing, three-level crushing be followed successively by coarse crushing, in it is broken and fine crushing, the coarse crushing uses jaw crusher, it is described in it is broken Pulverizer is covered using thunder, it is described fine crushing using tube mill；Partial size≤0.135mm coal gangue powder is ground into after gangue roasting Grain；The total mill is ground using high-frequency vibration, obtained after gangue powder and other raw material components, that is, auxiliary materials are ground altogether partial size≤ The mixed powder of 0.040mm；The mixed grind refers to that the water that its weight 5~20% is added in mixed powder or organic solvent pass through Mixing rolls to obtain ceramic material；It is described to loosen using Universalpulverizer, by the ceramic material after mixed grind in Universalpulverizer Wet fine silt is made；The balling-up uses disk balling machine, and wet fine silt generates ball in nodulizer；The first time screening Using the double-deck bushing screen, after ball is by screening, oversize returns to mixed grind process, and minus mesh enters nodulizer and is used as ball, sieves Middle material enters firing process；The firing uses rotary kiln or tunnel oven, and firing temperature is 1350 DEG C~1500 DEG C；The polishing It is that the ball after firing is carried out to itself grinding in tube mill；Second of screening is under condition of negative pressure with the double-deck bushing screen Polishing ball is sieved.
Technical effect of the invention is as follows: a kind of gangue proppant of the invention and preparation method thereof, in ceramic material Raw material components in using gangue roasting powder as major ingredient, instead of bauxite, be effectively utilized solid waste gangue, be coal Spoil again using providing new approach.Compared with the prior art the present invention, has the advantage that 1, technique uniqueness, is It is suitble to the advanced technology method of China's national situation, product quality maintains the leading position at home, is close to or up to the similar production in the U.S. Product have cost advantage outstanding and price advantage.2, it using disk balling machine, is pressed from both sides by specific rotation speeds and with horizontal plane at 60 ° Angle (inclination angle) setting, makes base ball make the continuous parabolic motion of three-dimensional space, and >=0.9, which is better than for the circularity of product, sphericity American-European similar product.3, yield is high, and low energy consumption, and every can produce qualified product 200kg per hour, only 1.1 kilowatts of power consumption.It 4, is China The approach kept away is opened in the development and utilization of gangue abundant.
Gangue proppant in high intensity manufactured by the present invention is with α-Al2O3(corundum) structure is principal crystalline phase, multicomponent oxygen After compound and mild-clay congruent melting with α-Al2O3It forms solid solution and glass phase and forms high-intensitive combination, hardness is only secondary In diamond.Product quality indicator are as follows: percentage of damage < 2~4%；Circularity, sphericity are >=0.9；Volume density≤1.65g/cm3；Depending on Density≤2.75g/cm3；Turbidity≤10FTU；During surface smoothness is；Acid solubility≤4.5%；Flow conductivity >=22.27 μ m2·cm。
Specific embodiment
Below with reference to examples illustrate the present invention.
The purpose of the present invention is the improvement to Selid propping agent process flow is produced using gangue as major ingredient, provide one kind Simple process, efficient, energy conservation, good product quality, at low cost, the preparation side of the gangue proppant in high intensity of suitable China's national situation Method.The technical scheme is that by major ingredient gangue after 1000 DEG C~1350 DEG C roasting temperatures, be ground into partial size≤ The powder of 0.135mm adds auxiliary material to wear into partial size≤0.040mm fine silt altogether, adds the water of 5~20% raw material weights or has Solvent progress mixed grind, uniformly mixes, and then passes through and loosens, balling-up (pelletizing), sieves and be burnt into (sintering).Mesh size is according to circle Depending on ball size requirements.
Concrete technology flow process is as follows: after the roasting of a. gangue, Al2O3Content be 55~70% (weight).B. auxiliary material is Many oxide Fe2O3、MgO、MnO2, clay and water.The weight proportion of major ingredient and auxiliary material is 85~95% and 5~15%.C. at Ball is carried out in the nodulizer that revolving speed is 10~50 revs/min and is installed with horizontal plane at 60 ° of angles.Globulation is to make first Raw material generates its partial size≤0.2mm ball (mother bulb) in nodulizer, powder-granule material is then gradually added again, regulation sphere diameter is made Ball.Screening after balling-up is enterprising in the double-deck bushing screen that upper aperture is 850 μm (20 mesh), lower aperture is 425 μm (40 mesh) Row.D. firing temperature is 1350 DEG C~1500 DEG C.
There are also polishings and screening process after the firing of above-mentioned process flow.Polishing is to carry out ball by tube mill Grinding between itself.Screening is under condition of negative pressure with 850 μm of aperture, the double-deck bushing screen in 425 μm of lower aperture or sieve pore evidence Depending on ball size requirements.Crushing after major ingredient roasting is successively to carry out carse, medium and small three-level crushing, the partial size after fine powder≤ 0.135mm.Various auxiliary materials and its weight content are Fe respectively2O32~10%, MgO 0.5~5%, MnO20.5~5% and viscous Soil 2~10%.Mill is to carry out ultra-fine grinding in high-frequency vibration mill altogether, altogether partial size≤0.015mm after mill.
A kind of gangue proppant, which is characterized in that the proppant is ceramic particle, and the ceramic particle is by gangue Ceramic material is fired, and the Coal gangue pottery porcelain pug refers in the raw material components of ceramic material is with gangue roasting powder Major ingredient.The gangue roasting powder content is 80wt%~95wt%.It include auxiliary material in the raw material components of the ceramic material, The auxiliary material includes clay and many oxide.The many oxide is Fe2O3, MgO and MnO2；The clay is soft viscous Soil.Fe2O3Feedstock Component content is 1wt%~15wt%, and MgO Feedstock Component content is 0.5wt%~10wt%, MnO2Raw material Constituent content is 0.5wt%~10wt%, and raw clay constituent content is 1wt%~10wt%.The gangue roasts powder Main chemical compositions and its weight content it is as follows: Al2O355~70%, SiO215~30%, Fe2O32~10.5%, TiO22~5.5%.The gangue proppant is with α-Al2O3(corundum) structure is principal crystalline phase, multi-component oxide and soft After clay congruent melting with α-Al2O3Form the combination of solid solution and glass phase, product quality indicator are as follows: percentage of damage < 2~4%；Circle Degree, sphericity are >=0.9；Volume density≤1.65g/cm3；Apparent density≤2.75g/cm3；Turbidity≤10FTU；During surface smoothness is； Acid solubility≤4.5%；Flow conductivity >=22.27 μm2·cm。
A kind of preparation method of gangue proppant, which is characterized in that including gangue roasting, crush, total mill, mixed grind system Ceramic material is obtained, loosened, balling-up, screening for the first time, firing, polished and sieve for the second time；The raw material group of the ceramic material Divide and content is as follows: it is 80wt%~95wt%, Fe that gangue, which roasts powder content,2O3Feedstock Component content be 1wt%~ 15wt%, MgO Feedstock Component content are 0.5wt%~10wt%, MnO2Feedstock Component content is 0.5wt%~10wt%, is glued Native Feedstock Component content is 1wt%~10wt%.The temperature of the gangue roasting is 1000 DEG C~1340 DEG C；The crushing is Multi-stage crushing, the multi-stage crushing are that three-level crushes, three-level crushing be followed successively by coarse crushing, in it is broken and fine crushing, the coarse crushing is adopted With jaw crusher, it is described in it is broken pulverizer is covered using thunder, it is described fine crushing to use tube mill；Partial size is ground into after gangue roasting The gangue powder of≤0.135mm；The total mill is ground using high-frequency vibration, by gangue powder and other raw material components, that is, auxiliary materials Partial size≤0.040mm mixed powder is obtained after mill altogether；The mixed grind refers to is added its weight 5~20% in mixed powder Water or organic solvent roll to obtain ceramic material by mixing；It is described to loosen using Universalpulverizer, it will in Universalpulverizer Wet fine silt is made in ceramic material after mixed grind；The balling-up uses disk balling machine, and wet fine silt generates circle in nodulizer Ball；The first time screening is using the double-deck bushing screen, and after ball is by screening, oversize returns to mixed grind process, and minus mesh enters Nodulizer is used as ball, and material enters firing process in sieve；The firing uses rotary kiln or tunnel oven, and firing temperature is 1350 DEG C ~1500 DEG C；The polishing is that the ball after firing is carried out to itself grinding in tube mill；Second of screening is negative Polishing ball is sieved with the double-deck bushing screen under the conditions of pressure.
Embodiment 1: raw material is made of major ingredient and auxiliary material.Major ingredient is gangue, main component and its content (weight) are as follows: Al2O365%, SiO218%, Fe2O33.55%, TiO23.33%, the type and content (weight) of auxiliary material is respectively Fe2O39%, MgO1.5%, MnO21.0%, mild-clay 4%.By major ingredient gangue after 1350 DEG C of roasting temperatures, successively It is fine crushing through broken and tube mill in jaw crusher coarse crushing, thunder illiteracy pulverizer, the fine powder of partial size < 0.088mm is obtained after screening.Later Add auxiliary material to grind (ultra-fine grinding) altogether, makes its fine powder partial size < 0.020mm.Then it sieves through balling-up, screening, firing and again, obtains To gangue proppant in high intensity finished product.Balling-up is in the nodulizer that at 60 ° of angles, revolving speed is 10~50 revs/min with horizontal plane Middle progress, process are so that powder is generated partial size≤0.2mm ball in nodulizer, then gradually add powder that sphere diameter < is made The ball of 1.0mm.Screening is using the double-deck bushing screen in 850 μm of upper aperture, 425 μm of lower aperture, and oversize returns to mixed grind process, Minus mesh enters nodulizer and is used as ball.Ball is calcined 2 hours in rotary kiln between 20/40 mesh, calcination temperature 1450 ℃.Polishing is that the ball after firing is carried out to itself grinding in tube mill.
Embodiment 2: bastard coal stone ore is ground into its partial size < 0.088mm's by carse, medium and small three-level after 1350 DEG C of roastings 4wt%Fe is added in powder2O3, 2wt%MgO, 4wt%MnO2Mixed oxide and 8wt% mild-clay, in high-frequency vibration Wear into partial size < 0.015mm fine silt in mill altogether, then plus the water of raw material weight 15% carry out mixed grind.By mixed grind at pug through ten thousand Energy pulverizer loosens into wet mash, at 60 ° of angles, is generating partial size in the nodulizer that revolving speed is 10~50 revs/min with horizontal plane The ball of < 0.2mm, then the ball that sphere diameter < 1.0mm is made in powder is gradually added.Manufactured ball by 850 μm of upper hole, The double-deck bushing screen in 425 μm of lower aperture is sieved, and ball returns to mixed grind process on sieve, is sieved lower ball return nodulizer and is made ball With.Ball of the sphere diameter between 20/40 mesh enters tunnel kiln sintering, and sintering temperature is 1400 DEG C, and sintering time is 3 hours.Finally, It will be qualified gangue proppant in high intensity finished product after same procedure polishing in the ball use-case 1 of firing and screening.
Product made by above-described embodiment, through pressing S.Y standard or A.P.1 standard detection, product quality indicator are as follows: broken Broken rate < 2~4%；Circularity, sphericity are >=0.9；Volume density≤1.65g/cm3；Apparent density≤2.75g/cm3；Turbidity≤10FTU； During surface smoothness is；Acid solubility≤4.5%；22.27 μm of flow conductivity2·cm。
It is hereby stated that described above facilitate those skilled in the art understand that the invention, but not limit the present invention The protection scope of creation.Any equivalent replacement described above, modification are improved without disengaging the invention substantive content And/or delete numerous conform to the principle of simplicity and the implementation that carries out, each fall within the protection scope of the invention.

Claims (7)

1. a kind of gangue proppant, which is characterized in that the proppant is ceramic particle, and the ceramic particle is by Coal gangue pottery Porcelain pug is fired, and the Coal gangue pottery porcelain pug refers in the raw material components of ceramic material based on gangue roasting powder Material；The raw material components and content of the ceramic material are as follows: it is 80wt%~95wt%, Fe that gangue, which roasts powder content,2O3It is former Material constituent content is 1wt%~15wt%, and MgO Feedstock Component content is 0.5wt%~10wt%, MnO2Feedstock Component content is 0.5wt%~10wt%, raw clay constituent content are 1wt%~10wt%.
2. a kind of gangue proppant according to claim 1, which is characterized in that the clay is mild-clay.
3. a kind of gangue proppant according to claim 1, which is characterized in that the gangue roasts the main of powder Chemical component and its weight content are as follows: Al2O355~70%, SiO215~30%, Fe2O32~10.5%, TiO22~ 5.5%.
4. a kind of gangue proppant according to claim 1, which is characterized in that the gangue proppant is with corundum α-the Al of structure2O3For principal crystalline phase, after multi-component oxide and mild-clay congruent melting with α-Al2O3Form solid solution and glass phase Combination, product quality indicator are as follows: percentage of damage < 4%；Circularity, sphericity are >=0.9；Volume density≤1.65g/cm3；Apparent density ≤2.75g/cm3；Turbidity≤10FTU；During surface smoothness is；Acid solubility≤4.5%；Flow conductivity >=22.27 μm2·cm。
5. a kind of preparation method of gangue proppant, which is characterized in that including gangue roasting, crushing, mill, mixed grind are made altogether Ceramic material loosens, balling-up, screening for the first time, firing, polishes and sieve for the second time；The raw material components of the ceramic material And content is as follows: it is 80wt%~95wt%, Fe that gangue, which roasts powder content,2O3Feedstock Component content be 1wt%~ 15wt%, MgO Feedstock Component content are 0.5wt%~10wt%, MnO2Feedstock Component content is 0.5wt%~10wt%, is glued Native Feedstock Component content is 1wt%~10wt%.
6. a kind of preparation method of gangue proppant according to claim 5, which is characterized in that the gangue roasting Temperature be 1000 DEG C~1340 DEG C；Described crush is multi-stage crushing, and the multi-stage crushing is three-level crushing, and the three-level crushes Be followed successively by coarse crushing, in it is broken and fine crushing, the coarse crushing use jaw crusher, it is described in it is broken using thunder cover pulverizer, it is described fine crushing Using tube mill；Partial size≤0.135mm gangue powder is ground into after gangue roasting；The total mill uses high-frequency vibration Mill obtains partial size≤0.040mm mixed powder after grinding gangue powder and other raw material components, that is, auxiliary materials altogether；The mixed grind Refer to that the water that its weight 5~20% is added in mixed powder or organic solvent roll to obtain ceramic material by mixing；It is described It loosens using Universalpulverizer, wet fine silt is made in the ceramic material after mixed grind in Universalpulverizer.
7. a kind of preparation method of gangue proppant according to claim 6, which is characterized in that the balling-up is using circle Disk nodulizer, wet fine silt generate ball in nodulizer；Using the double-deck bushing screen, ball passes through screening for the first time screening Afterwards, oversize returns to mixed grind process, and minus mesh enters nodulizer and is used as ball, and material enters firing process in sieve；The firing Using rotary kiln or tunnel oven, firing temperature is 1350 DEG C~1500 DEG C；The polishing is ball after being burnt into tube mill It is middle to carry out itself grinding；Second of screening is sieved with the double-deck bushing screen to polishing ball under condition of negative pressure.
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CN106967408B (en) * 2017-03-28 2019-11-15 太原理工大学 A kind of ultra-low-density ceramic proppant and preparation method thereof
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CN112374865B (en) * 2020-11-25 2022-04-12 江苏金石研磨有限公司 Ceramic grinding ball made of zircon tailings and coal gangue and preparation method thereof
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