CN103159464B - Method for preparing fracturing propping agent for shale gas exploitation by utilizing slag - Google Patents
Method for preparing fracturing propping agent for shale gas exploitation by utilizing slag Download PDFInfo
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- CN103159464B CN103159464B CN201310130487.0A CN201310130487A CN103159464B CN 103159464 B CN103159464 B CN 103159464B CN 201310130487 A CN201310130487 A CN 201310130487A CN 103159464 B CN103159464 B CN 103159464B
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Abstract
The invention discloses a method for preparing a fracturing propping agent for shale gas exploitation by utilizing slag. According to the method, slag serves as a main material, and high-temperature alumina dust collecting powder, alumina powdered waste and spodumene tailings form a composite sintering aid, wherein the slag is high in carbon content, lots of gas can be generated inside a propping agent when carbon is burnt at a high temperature, and the gas is closed in the local area of small granules of the propping agent by utilizing a high-viscosity liquid phase generated by the sintering aid, so that massive distributed tiny closed pores can be formed to achieve the effects of reducing density and increasing pressure resistance. According to the method, the used slag and the adopted composite sintering aid are waste materials, so that natural resources can be saved favorably, the technical content and additional value of the product can be increased, and the economical benefit can be improved.
Description
Technical field
The present invention relates to the special-purpose pressure break production technique of shale gas field, be specifically related to a kind of slag that utilizes and prepare the method for fracturing propping agents for shale gas exploitation.
Background technology
Shale gas permeability of reservoir is low, and the resistance ratios conventional gas of air-flow is large, and exploitation difficulty is larger, and the ultimate recovery factor of shale gas depends on effective fracturing methods, and wherein the effect of fracturing propping agents is very important.Natural sand or the artificial stays agent three types of the main natural siliceous sand of now widely used propping agent, artificial porcelain granule and coating Procuring coating and curable coating resin.Wherein mainly to adopt bauxitic clay be raw material to artificial porcelain granule propping agent.With the exhaustion of fine aluminum alumina resource, people start with low-grade bauxitic clay and other aluminum-containing raw material.
Application number is that 201210453012.0 Chinese patents disclose a kind of extremely-low density ceramsite propping agent and preparation method thereof, this low-density ceramic proppant be take bauxite as main raw material, allocate clay, quartz, rhombspar into, with manganese ore and add a kind of in a small amount of titanium dioxide, calcium carbonate, ferric oxide or be combined as sintering agent, through ball milling, granulation, burn till, sieve and obtain finished product.Application number is that 201210116790.0 Chinese patents disclose a kind of production technique of utilizing low-grade bauxite to prepare ceramsite propping agent, and major ingredient is low-grade bauxite, adds kaolin, take ilmenite concentrate as sintering agent.
Utilize other solid waste to prepare propping agent and can reduce the dependence to bauxitic clay.As Chinese patent 201010301161 discloses a kind of haydite and preparation method thereof, its raw material and component thereof are: aluminous fly-ash or slag 40%-99.5%, binding agent 0.5-60%, particularly also add the feed composition of subsidiary material 1-23%.Patent 201010550527 discloses a kind of preparation method of haydite, and it is by the broken powder that obtains of flyash, kaolin, ferric oxide and magnesium basic carbonate wet-milling post-drying; After powder is made to spheroidal particle, biscuiting obtains biscuiting haydite; Get Li-Al-Si system glass ceramics powder; Prepared microcrystalline glass powder is poured in tablets press and stirred, after biscuiting haydite surface is wrapped up completely by microcrystalline glass powder, must wrap up the biscuiting haydite of microcrystalline glass powder; The biscuiting haydite of parcel microcrystalline glass powder is put into tablets press, add powder, must haydite be burnt after the biscuiting haydite that has a microcrystalline glass powder to be wrapped is wrapped up completely by powder again; In retort furnace, after sintering, fragmentation obtains haydite.Chinese patent 200910015979 discloses a kind of high-strength compress supporting agent for coarse oil and preparation method thereof, and it adopts ceramic rod waste material, red mud, flyash is main raw material, and interpolation rhombspar, ceramic clay are auxiliary material, and manganese oxide or barium carbonate are sintering agent.But it is less to utilize slag to prepare the report of haydite.As: the Chinese patent that application number is 201110237966.3 discloses a kind of material prescription and haydite production method thereof of gasifier slag haydite, and wherein gasifier slag is main raw material, is also added with CaO, CaSO
4or glass powder is solubility promoter.Gained haydite particle diameter large (10mm), intensity is low, for filter tank filler and building heat preservation, but cannot be as shale gas exploitation fracturing propping agents.This is because the particle diameter little (its particle requirement granularity is 1-500 micron) of the fracturing propping agents that shale gas exploitation needs, and therefore above-mentioned haydite cannot be as the special-purpose fracturing propping agents of shale gas.In addition, how in propping agent small-particle, forming more equally distributed pore is also a difficult problem.
Sintering agent is also that artificial porcelain granule propping agent is produced requisite.Chinese patent 200510021256 provides a kind of high titanium type petroleum oil pressing crack propping agent, and its chemical composition forms and comprises by weight percentage: 5～45% high-titanium blast furnace slag, 10～30% high alumina brick, 17～77% bauxitic clays and 4～8% Composite sintering agent.Application number is that 201210143576 Chinese patent discloses a kind of extremely-low density ceramsite propping agent that pebbles is main additive and preparation method thereof that utilizes.Selecting potassium felspar sand, calcite and magnesia is sintering agent, lower than the cost of at present conventional manganese ore powder.The Chinese patent that application number is 201110236846 provides a kind of preparation method of lightweight acidproof ceramic fracturing propping agent, and its sintering agent used is one or more in the compound of barium, calcium, magnesium and boron; Application number is that 201010143771 Chinese patent discloses a kind of preparation method without silicon or low-silicon acidproof ceramic fracturing propping agent, and the sintering agent that it uses is one or more in titanium dioxide, boric acid, calcium carbonate, magnesium oxide and rhombspar; Application number is the preparation method that 200710168057 Chinese patent discloses a kind of acid-resistant pressing crack supporting agent, and its sintering agent used helps and burns for Fe
2o
3, TiO
2, one or several in borax and magnetite.Above sintering agent cost is higher.
Summary of the invention
The present invention has overcome above-mentioned the deficiencies in the prior art, a kind of method of fracturing propping agents for shale gas exploitation of preparing is provided, the method is that the slag of take after coal combustion is main raw material, can utilize the characteristic that boiler slag carbon content is high completely, in propping agent high temperature production process, slag residual carbon burns away, the a large amount of gases that produce, the sintering agent that utilizes special preparation, allows gas local tiny area in the very little propping agent of particle size become sealed porosity, thereby is conducive to reduce propping agent density.
Technical scheme of the present invention is: a kind of slag that utilizes is prepared the method for fracturing propping agents for shale gas exploitation, it is characterized in that, take slag as major ingredient, with gather dust powder (the useless dirt powder of collecting while being high temperature alumina power production), alumina powder jointed waste material (containing sodium 0.5～1.5wt%) and triphane mine tailing of high temperature alumina, form complex sintering aids, the weight part of each raw material is as follows: 88.5～93.8 parts, slag, gather dust 5～8 parts, powder of high temperature alumina, 1～2 part, alumina powder jointed waste material, 0.2～1.5 part of triphane mine tailing.
After described slag is producer gas generator gasified raw material coal, the solid residue of acquisition, its chemical constitution and mass percent thereof are: SiO
244-48%, Al
2o
330-34%, Fe
2o
3≤ 5.5%, CaO≤5.5%, all the other are carbon and inevitable impurity;
Described triphane mine tailing containing lithium amount be 3-4wt%.
The gather dust alumina content of powder and alumina powder jointed waste material of described high temperature alumina is 90～95%(mass ratio).
Preparation method of the present invention is conventional preparation method, preferably adopts Chinese patent 201210116790.0(denomination of invention: utilize low-grade bauxite to prepare the production technique of ceramsite propping agent) in preparation method.
Boiler slag carbon content of the present invention is >=10%, utilizes burning under carbon high-temp at a large amount of gas of the inner generation of propping agent, to utilize the high viscosity liquid phase of sintering agent generation, by gas sealing and regional area, form a large amount of small closed pore that distributes, play reduction density, increase measuring body effect.
Gather dust powder and alumina powder jointed waste material (containing sodium 0.5～1.5) and triphane mine tailing when described complex sintering aids is high temperature alumina.The fusing assistant effect of the sodium that utilizes lithium in triphane mine tailing and alumina powder jointed waste material and gather dust in powder forms liquid phase when propping agent burns till.The utilization powder particles that gathers dust is thin, and the feature that alumina content is high increases the viscosity of liquid phase, thereby is conducive to seal up the gas that in slag, carbon burning produces.In addition, this sintering agent all adopts waste material, and both utilization of waste material have solved again scrap materials of enterprises pollution problem.
The special-purpose fracturing propping agents of shale gas of the present invention are according to SY/T5108-2006, " fracturing propping agents performance test recommend method " tested, and test result is: extremely-low density, special-purpose fracturing propping agents (20-40 order): the volume density≤1.45g/cm of high strength shale gas
3; Volume density≤2.65g/cm
3; 52MPa locking pressure percentage of damage 2.2～3%; 69MPa locking pressure percentage of damage 5～6%; Acid resistance < 3%.
The present invention compared with prior art, has following outstanding feature:
(1) slag used in the present invention is all waste material with the composite sintering adopting, and contributes to save natural resource, has increased technology content and the added value of product, increases economic efficiency.
(2) boiler slag carbon content of the present invention is high, utilizes burning under carbon high-temp at a large amount of gas of the inner generation of propping agent, to utilize the high viscosity liquid phase of sintering agent generation, by gas sealing and regional area, form a large amount of small closed pore that distributes, play reduction density, increase measuring body effect.
Embodiment
Embodiment is only described further the present invention, but is not limited only to this.
Embodiment 1:
Proportioning (weight part): 92 parts, slag, gather dust 6 parts, powder of high temperature alumina, 1 part, alumina powder jointed waste material, 1 part of triphane mine tailing.
The chemical constitution of described slag and mass percent thereof are: SiO
244%, Al
2o
333%, Fe
2o
35%, CaO5%;
Described triphane mine tailing containing lithium amount be 3.8wt%.
The gather dust alumina content of powder and alumina powder jointed waste material of described high temperature alumina is 90～95%(mass ratio); Wherein alumina powder jointed waste material is containing sodium 0.5-1.5%(mass ratio).
Preparation method of the present invention adopts Chinese patent 201210116790.0(denomination of invention: utilize low-grade bauxite to prepare the production technique of ceramsite propping agent) in preparation method.
Specific as follows: major ingredient bauxitic clay ore and slag to be broken for after the particle of 5mm, to be mixed into compound with other auxiliary materials.With compound: after the weight ratio of alumina balls grinding medium: water=1:2.5:0.9 is mixed, add the Sodium hexametaphosphate 99 ball-milling additive of mixture quality 0.6%, being placed in ball mill wet-milling becomes mud in 18 hours, makes mud granularity reach 13 microns, puts into suction pit old.Old rear gained slush pump spraying is dry, and to obtain moisture content be 4% discrete particle; Then above-mentioned discrete particle is broken up again to the broken powder for 13 microns of particle diameters; After above-mentioned gained powder is put in storage, proceed in disk pelletizing machine, under the unidirectional uniform rotation of nodulizer, with water spray rolling granulation, particle obtains work in-process base ball through screening; Then work in-process base ball is sent into and dried-burn till in system ensemble, at 1330 ℃, soaking time obtains finished product for 3 hours, and finished product is carried out to polished finish, increases the surface flatness of propping agent haydite.
According to oil and gas industry standard < < fracturing propping agents performance test recommend method > > SY/T5108-2006, the fracturing propping agents of the present embodiment 1 preparation are tested, main performance index are in Table 1.
Embodiment 2:
Proportioning (weight part): 88.5 parts, slag, gather dust 8 parts, powder of high temperature alumina, 2 parts, alumina powder jointed waste material, 1.5 parts of triphane mine tailings.
The chemical constitution of described slag and mass percent thereof are: SiO
244.8%, Al
2o
333.8%, Fe
2o
34.8%, CaO5.3%.
The performance index of other raw materials and preparation method are with embodiment 1, according to oil and gas industry standard < < fracturing propping agents performance test recommend method > > SY/T5108-2006, the fracturing propping agents of the present embodiment 2 preparations are tested, main performance index are in Table 1.
Embodiment 3
Proportioning (weight part): 93.5 parts, slag, gather dust 5 parts, powder of high temperature alumina, 1 part, alumina powder jointed waste material, 0.5 part of triphane mine tailing.
The chemical constitution of described slag and mass percent thereof are: SiO
244.3%, Al
2o
333.7%, Fe
2o
35.0%, CaO5.2%.
The performance index of other raw materials and preparation method are with embodiment 1, according to oil and gas industry standard < < fracturing propping agents performance test recommend method > > SY/T5108-2006, the fracturing propping agents of the present embodiment 3 preparations are tested, main performance index are in Table 1.
The performance index of ceramsite propping agent prepared by embodiment 1-3
Claims (3)
1. one kind is utilized slag to prepare the method for fracturing propping agents for shale gas exploitation, it is characterized in that, take slag as major ingredient, with gather dust powder, alumina powder jointed waste material and triphane mine tailing of high temperature alumina, form complex sintering aids, the weight part of each raw material is as follows: 88.5～93.8 parts, slag, gather dust 5～8 parts, powder of high temperature alumina, 1～2 part, alumina powder jointed waste material, 0.2～1.5 part of triphane mine tailing; The chemical constitution of described slag and mass percent thereof are: SiO
244-48%, Al
2o
330-34%, Fe
2o
3≤ 5.5 %, CaO≤5.5%, carbon content is>=10%; Described alumina powder jointed waste material is containing sodium 0.5 ~ 1.5wt%.
2. a kind of slag that utilizes as claimed in claim 1 is prepared the method for fracturing propping agents for shale gas exploitation, it is characterized in that, the gather dust alumina content of powder and alumina powder jointed waste material of described high temperature alumina is 90 ~ 95wt%.
3. a kind of slag that utilizes as claimed in claim 1 or 2 is prepared the method for fracturing propping agents for shale gas exploitation, it is characterized in that, described triphane mine tailing containing lithium amount, be 3-4wt%.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555316B (en) * | 2013-10-29 | 2016-07-13 | 孝义市鑫腾矿业有限公司 | A kind of shale oil-gas mining pressure break ceramsite propping agent and manufacture method thereof |
| CN104830308B (en) * | 2015-05-29 | 2017-08-25 | 河南天祥新材料股份有限公司 | Shale gas exploitation fracturing propping agents and preparation method thereof |
| CN105505362A (en) * | 2015-12-02 | 2016-04-20 | 中国石油天然气股份有限公司 | Selective water-blocking, oil-permeable and sand-preventing proppant as well as preparation method and application thereof |
| CN107011886B (en) * | 2017-04-10 | 2019-09-13 | 中国铝业股份有限公司 | A kind of method that mineral processing tailing of bauxite prepares ceramsite propping agent |
| CN107445484B (en) * | 2017-09-12 | 2020-03-27 | 福建省德化县华茂陶瓷有限公司 | Bark glaze, bark glaze ceramic product prepared from bark glaze and preparation method of bark glaze ceramic product |
| CN111454076B (en) * | 2020-04-30 | 2022-07-12 | 西安建筑科技大学 | Ceramsite proppant prepared from blast furnace tapping channel waste and preparation process |
| CN114057492B (en) * | 2021-11-26 | 2022-11-15 | 江苏科技大学 | Beta' -Sialon-AlN-TiC composite ceramic material and preparation method thereof |
| CN114015431B (en) * | 2021-12-07 | 2023-01-31 | 河南郑矿机器有限公司 | Low-density petroleum ceramsite proppant and preparation method thereof |
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| RU2383578C2 (en) * | 2007-09-18 | 2010-03-10 | Шлюмберже Текнолоджи Б.В. | Proppant, method of production and method of hydraulic break of formation using produced proppant |
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Patent Citations (4)
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| CN101786845A (en) * | 2010-02-03 | 2010-07-28 | 四川省鑫沙矿渣微粉有限责任公司 | Ceramsite and production method thereof |
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| CN102876315A (en) * | 2012-10-13 | 2013-01-16 | 山西方兴耐火材料有限公司 | Low-density ceramsite supporting agent and preparation method thereof |
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