CN104628410A - Method for preparing porous mullite microspheres - Google Patents
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- CN104628410A CN104628410A CN201510032161.3A CN201510032161A CN104628410A CN 104628410 A CN104628410 A CN 104628410A CN 201510032161 A CN201510032161 A CN 201510032161A CN 104628410 A CN104628410 A CN 104628410A
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- oil
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Abstract
The invention relates to a technology for molding a ceramic material and particularly relates to a method for preparing porous mullite microspheres. The method comprises the following steps of mixing kaolin, bauxite, a crystalline catalyst AlF3 and a sintering aid to obtain a uniform mixed powder; adding a dispersant to the mixed powder prepared in the step 1 and adding deionized water to prepare uniform and stable water-based ceramic slurry with different solid contents, pouring the slurry into oil, forming balls and emulsifying the water-based ceramic slurry and oil in a polystyrene tray under the action of high-speed stirring, placing the mixed solution of slurry and oil into the polystyrene tray, freezing and filtering to obtain solidified ceramic microspheres, drying the solidified ceramic microspheres and carrying out pressureless sintering on dried ceramic microspheres in an aluminum oxide crucible to obtain the porous mullite microspheres. By the method, the ceramsite density is decreased and meanwhile the production cost is reduced and the method is used for preparing high-strength low-density ceramic for oil fracturing exploitation.
Description
Technical field
The present invention relates to a kind of forming technique of stupalith, specifically a kind of preparation method of porous mullite microballoon.
Technical background
Oil, also known as crude oil, is thick, the Vandyke brown liquid of one of mixture composition of various alkane, naphthenic hydrocarbon, aromatic hydrocarbon.In recent years, along with the fast development of Chinese national economy, the demand of oil day by day strengthens, and improves the utilization ratio in exploitation oil field, reduces the cost of winning of oil, becomes the important subject urgently to be resolved hurrily that China's current oil production industry faces.In recent years, in the new proven reserve of China's oil about 82% be hyposmosis storage.Most Oil/gas Well must utilize fracturing yield increasing technology to improve Oil & Gas Productivity.
Hydraulic fracturing technology is one of important technology improving Oil & Gas Productivity in petroleum industry.In hydraulic fracturing process, be the state making waterfrac treatment rock fracture fracture width keep wider, the optional spherical solid particles with having advantages of higher compressive strength injects rock crevice supporting crack with fracturing liquid.Selected propping agent propping agent improves the flow conductivity near wellbore stratum in rock crevice, reduces liquid is flowed into pit shaft resistance by stratum, adds Oil/gas Well output.
Quartz sand is widely used in oil-gas field fracturing exploitation as hydraulic fracturing proppants.Volume density is 1.62g/cm
3; Volume density is 2.62g/cm
3; Under 28MPa locking pressure, percentage of damage is 12.0% ~ 14.0%.In the eighties in 20th century, going abroad has showed precured resin coated quartz sand outward.It is, the deficiency such as flow conductivity poor low according to quartz sand ultimate compression strength, at quartz sand surface overlay film one deck thermosetting resin, and the Novel propping agent solidified under certain condition, for pressure break supporting crack, replace quartz sand and part haydite.
In recent years, many scientific researchers, in order to prepare cheap high performance bauxitic clay base petroleum fracturing propping agent, had carried out many Science Explorationss.Such as, in sintering process, introducing some mineral additives to promote to be formed more corundum phase or mullite phase, taking to reduce costs other technologies to innovate improvement of production process etc.Develop the use that sintering ceramsite meets most Oil/gas Well substantially
At present, in Oil/gas Well, in waterfrac treatment volume increase, mainly use the petroleum fracturing propping agent of the low-density propping agent of natural siliceous sand, medium tenacity, medium tenacity high density proppants, high-intensity high-density propping agent and coating Procuring coating and five types such as the natural sand of curable coating resin or artificial stays agent.They play different effects separately in oil gas well mining process.
For the ease of pumping into down-hole, reduce propping agent to the wearing and tearing of equipment, therefore when withstanding formation closure pressure, the density of propping agent is more low better.Be under the condition of 200 DEG C in temperature, proppant particles not with the reservoir fluid generation chemical reaction of fracturing liquid and oil gas rock crevice, in current industry, the acid solubility permissible value of common demands propping agent is not higher than 7%.There is the sufficient source of goods, cheap price.
Summary of the invention
Technical problem to be solved by this invention is: how to reduce production cost, is preparing porous mullite haydite simultaneously, is reducing its density, obtain can be used for oil fracturing, high-strength low close porous mullite haydite.
The technical solution adopted in the present invention is: a kind of preparation method of porous mullite microballoon, carries out according to following step:
Step one, by kaolin, bauxitic clay, crystalline catalysts AlF
3,sintering aid mixes
By kaolin, bauxitic clay according to after mass percent 2.1:1 ~ 3:1 mixing, add crystalline catalysts AlF
3, then (sintering aid is MgO, TiO to add sintering aid
2, MoO
3in any one, if sintering aid is MgO, MgO quality account for 4.62% of mixture total mass, if sintering aid is TiO
2, TiO
2quality accounts for 9.14% of mixture total mass, if sintering aid is MoO
3, MoO
3quality accounts for the 16.5wt% of mixture total mass), wherein AlF
3quality account for 4% ~ 8% of mixture total mass, and with Si
3n
4ball and dehydrated alcohol are ball-milling medium, continuous ball milling wet mixing 20h, then dry and sieve, obtain uniform mixed powder;
Dispersion agent (dispersion agent for polyvinyl alcohol or polyvinyl alcohol) is added in step 2, the mixed powder prepared in step one, and then add deionized water, be placed in ball grinder ball milling 8 h ~ 24h, prepare the uniform and stable aqueous-based ceramic slurry of different solid load, wherein dispersion agent accounts for 0.5% ~ 1% of mixed powder quality, and the volume of slurry solid phase accounts for 10% ~ 40% of slip cumulative volume;
Step 3, slurry to be poured in oil into the (mixture that oil is Semen Maydis oil and kerosene, its mass ratio is 3:2 ~ 10:1), aqueous-based ceramic slurry and oil balling-up emulsification under the effect of high-speed stirring (high-speed stirring refers to that mixing speed is 200 ~ 250 revs/min) in polystyrene dish, form oil-slurry mixed solution, aqueous-based ceramic slurry forms microspheric drop;
Step 4, oil-slurry mixed solution is put into polystyrene dish, alcohol medium in freezing (freezing temp is-30 DEG C ~-10 DEG C), and filter the ceramic microsphere and separation of oil that make to solidify;
Step 5, ceramic microsphere will be solidified be placed in freeze drier, and make it dry; Dried ceramic microsphere is carried out in alumina crucible pressureless sintering and form porous mullite microballoon, non-pressure sintering technology is for being that 20 DEG C/min is warming up to 950 DEG C with temperature rise rate, insulation 1h, is then warming up to 1100 DEG C ~ 1300 DEG C, and insulation 2h obtains porous mullite microballoon.
The invention has the beneficial effects as follows: the present invention breaks through traditional technology, adopting eco-friendly water for preparing slurry; Adopt the Technology that in oil, balling-up combines with lyophilize to prepare the porous mullite microballoon with high porosity, porous mullite microsphere density is less than 1.6g/cm
3, and there is suitable ultimate compression strength.The present invention adopt main raw material be kaolin to replace bauxitic clay, and adopt novel forming technology to prepare porous mullite haydite, reduce haydite density, reduce production cost simultaneously, prepare the high-strength low close pottery for oil fracturing exploitation.
Accompanying drawing explanation
Fig. 1 is the microstructure SEM photo of porous mullite microballoon.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Specific embodiments one: in the present embodiment, the preparation of porous mullite haydite realizes according to the following steps: one, configure for the preparation of the starting powder kaolin of mullite, bauxitic clay by percent mass 2.1:1, and with crystalline catalysts AlF
3(massfraction is 4% of mixture), sintering aid are MgO(massfraction is 4.62% of mixture) mix with Si
3n
4ball and dehydrated alcohol are ball-milling medium, continuous ball milling wet mixing 20h; Then dry and sieve, obtain uniform mixed powder; Two, by deionized water, dispersion agent (0.5-1% of mixed powder quality) and mixed powder (fractional solid volume is 10-40vol%) are placed in ball grinder ball milling 8h, prepare the uniform and stable water-based slurry of different solid load; Three, pour in oil phase by stable slurry, aqueous-based ceramic slurry and oil phase be balling-up emulsification under the effect of high-speed stirring in polystyrene dish, prepares microspheric drop with this; Four, simultaneously, by freezing in the alcohol medium of-30 DEG C for the polystyrene dish that the oil after emulsification-slurry mixed solution is housed, and the ceramic microsphere and separation of oil that make to solidify is filtered; Five, the sample solidified is placed in freeze drier, make it dry, the time is 48h; Six, haydite complete for drying is carried out pressureless sintering in alumina crucible.
Embodiment two: present embodiment and embodiment one are unlike the crystalline catalysts AlF in step one
3massfraction be 8wt%.Other steps are identical with embodiment one with parameter.
Embodiment three: present embodiment and embodiment one are TiO unlike the employing sintering aid in step one
2(massfraction is the 9.14wt% of mixture).Other steps are identical with embodiment one with parameter.
Embodiment four: present embodiment and embodiment one are MoO unlike the employing sintering aid in step one
3(massfraction is the 16.5wt% of mixture).Other steps are identical with embodiment one with parameter.
Embodiment five: present embodiment and embodiment one to four are the slurry that (9:1,8:2,7:3,6:4) prepares different solid load unlike the volume ratio of water in step 2 and starting powder.Other steps are identical with one of embodiment one to four with parameter.
Embodiment six: present embodiment and embodiment one to five are polyvinyl alcohol or polyvinyl alcohol unlike dispersion agent in the preparation process of slurry in step 2, and other steps are identical with one of embodiment one to three with parameter.
Embodiment seven: present embodiment and embodiment one to five are 0.5wt% or 1wt% of mixed powder unlike the amount of dispersion agent in the preparation process of slurry in step 2, and other steps are identical with one of embodiment one to five with parameter.
Embodiment eight: present embodiment and embodiment one to seven are placed in ball grinder ball milling 24h or 12h unlike mixture in step 2, and other steps are identical with one of embodiment one to six with parameter.
Embodiment nine: present embodiment and embodiment one to eight are the mixture of Semen Maydis oil and kerosene unlike oil phase used in step 3, and its mass ratio is respectively (10:1; 8:2; 6:4).Other steps are identical with one of embodiment one to seven with parameter.
Embodiment ten: present embodiment and embodiment one to eight are respectively 200,220,250 R/min unlike mixing speed used in step 3.Other steps are identical with one of embodiment one to seven with parameter.
Embodiment 11: present embodiment and embodiment one to ten realize radial freezing unlike being immersed completely in low-temperature receiver by it by the polyethylene mould pouring slurry in step 4, and freezing temp is respectively-10 DEG C ,-30 DEG C.Other steps are identical with one of embodiment one to seven with parameter.
Embodiment 12: sample complete for drying is placed in alumina crucible pressureless sintering unlike in step 6 by present embodiment and embodiment one to ten one, be that 20 DEG C/min is warming up to 950 DEG C with temperature rise rate, insulation 1h, finally be warming up to 1100 DEG C, insulation 2h obtains porous mullite haydite, and other steps are identical with one of embodiment one to ten one with parameter.
Embodiment 13: sample complete for drying is placed in alumina crucible pressureless sintering unlike in step 6 by present embodiment and embodiment one to ten one, be that 20 DEG C/min is warming up to 950 DEG C with temperature rise rate, insulation 2h, finally be warming up to 1200 DEG C, insulation 2h obtains porous mullite haydite, and other steps are identical with one of embodiment one to ten one with parameter.
Embodiment 14: sample complete for drying is placed in alumina crucible pressureless sintering unlike in step 4 by present embodiment and embodiment one to ten one, be that 20 DEG C/min is warming up to 950 DEG C with temperature rise rate, insulation 2h, finally be warming up to 1300 DEG C, insulation 2h obtains porous mullite haydite, and other steps are identical with one of embodiment one to ten one with parameter.
Above embodiment can prepare the finished product porous mullite microballoon, and is all the porous mullite microballoon of high porosity, and porous mullite microsphere density is less than 1.6g/cm
3, and there is suitable ultimate compression strength.
Claims (7)
1. a preparation method for porous mullite microballoon, is characterized in that carrying out according to following step:
Step one, by kaolin, bauxitic clay, crystalline catalysts AlF
3,sintering aid mixes
By kaolin, bauxitic clay according to after mass percent 2.1:1 ~ 3:1 mixing, add crystalline catalysts AlF
3, then add sintering aid, wherein AlF
3quality account for 4% ~ 8% of mixture total mass, and with Si
3n
4ball and dehydrated alcohol are ball-milling medium, continuous ball milling wet mixing 20h, then dry and sieve, obtain uniform mixed powder;
Step 2, step one prepare mixed powder in add dispersion agent, and then add deionized water, be placed in ball grinder ball milling 8 h ~ 24h, prepare the uniform and stable aqueous-based ceramic slurry of different solid load, wherein dispersion agent accounts for 0.5% ~ 1% of mixed powder quality, and the volume of slurry solid phase accounts for 10% ~ 40% of slip cumulative volume;
Step 3, pour in oil by slurry, aqueous-based ceramic slurry and oil balling-up emulsification under the effect of high-speed stirring in polystyrene dish, form oil-slurry mixed solution, aqueous-based ceramic slurry forms microspheric drop;
Step 4, oil-slurry mixed solution is put into polystyrene dish, alcohol medium in freezing, and filter the ceramic microsphere and separation of oil that make to solidify;
Step 5, ceramic microsphere will be solidified be placed in freeze drier, and make it dry; Dried ceramic microsphere is carried out in alumina crucible pressureless sintering and form porous mullite microballoon.
2. the preparation method of a kind of porous mullite microballoon according to claim 1, is characterized in that: step is a kind of, and sintering aid is MgO, TiO
2, MoO
3in any one, if sintering aid is MgO, MgO quality account for 4.62% of mixture total mass, if sintering aid is TiO
2, TiO
2quality accounts for 9.14% of mixture total mass, if sintering aid is MoO
3, MoO
3quality accounts for the 16.5wt% of mixture total mass.
3. the preparation method of a kind of porous mullite microballoon according to claim 1, is characterized in that: the dispersion agent described in step 2 for polyvinyl alcohol or polyvinyl alcohol.
4. the preparation method of a kind of porous mullite microballoon according to claim 1, it is characterized in that: the oil in step 3 is the mixture of Semen Maydis oil and kerosene, its mass ratio is 3:2 ~ 10:1.
5. the preparation method of a kind of porous mullite microballoon according to claim 1, is characterized in that: the high-speed stirring in step 3 refers to that mixing speed is 200 ~ 250 revs/min.
6. the preparation method of a kind of porous mullite microballoon according to claim 1, is characterized in that: the freezing temp in step 4 is-30 DEG C ~-10 DEG C.
7. the preparation method of a kind of porous mullite microballoon according to claim 1, it is characterized in that: in step 5, non-pressure sintering technology is for being that 20 DEG C/min is warming up to 950 DEG C with temperature rise rate, insulation 1h, is then warming up to 1100 DEG C ~ 1300 DEG C, and insulation 2h obtains porous mullite microballoon.
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| CN104628410B CN104628410B (en) | 2016-05-25 |
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Cited By (14)
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|---|---|---|---|---|
| CN105274623A (en) * | 2015-10-27 | 2016-01-27 | 天津大学 | Method for in-situ growth of mullite whiskers by virtue of vacuum impregnation and freeze drying |
| CN105347775A (en) * | 2015-12-08 | 2016-02-24 | 太原理工大学 | Preparation method of porous mullite ceramic applicable to diesel particulate filter |
| CN105399401A (en) * | 2015-11-10 | 2016-03-16 | 太仓捷公精密金属材料有限公司 | Ceramic metal material |
| CN106244135A (en) * | 2016-08-12 | 2016-12-21 | 郑州市少林滤材有限公司 | A kind of ceramsite propping agent compositions and its preparation method and application |
| CN106278349A (en) * | 2016-08-10 | 2017-01-04 | 袁春华 | A kind of preparation method of low-density and high-strength polymer-coated ceramic powder proppant |
| CN108484201A (en) * | 2018-06-14 | 2018-09-04 | 哈尔滨工业大学 | A kind of low-shrinkage porous silicon nitride ceramic and preparation method thereof |
| CN108854946A (en) * | 2018-06-07 | 2018-11-23 | 太原理工大学 | A kind of hierarchical porous structure zeolite absorption/catalyst and its construction method |
| CN110903094A (en) * | 2019-12-25 | 2020-03-24 | 苏州纳迪微电子有限公司 | Spherical aluminum nitride and preparation method and application thereof |
| CN111559918A (en) * | 2020-05-27 | 2020-08-21 | 中国科学院上海硅酸盐研究所 | Method for preparing porous ceramic body by combining microemulsion with freeze drying |
| CN111763080A (en) * | 2020-06-22 | 2020-10-13 | 深圳市东有新材料科技有限公司 | Hollow mullite microspheres and preparation method thereof |
| CN112811920A (en) * | 2021-02-09 | 2021-05-18 | 新沂北美高科耐火材料有限公司 | Ultrahigh-temperature refractory composite material and preparation method thereof |
| CN114572990A (en) * | 2022-03-15 | 2022-06-03 | 太原理工大学 | Preparation method of calcined kaolin with high oil absorption value |
| CN114853498A (en) * | 2022-04-22 | 2022-08-05 | 胜利油田新海兴达实业集团有限责任公司 | Micron ceramic ball material and preparation method and application thereof |
| CN115403364A (en) * | 2022-09-09 | 2022-11-29 | 天津大学 | Method for preparing columnar mullite by using rapid sintering process after pretreatment of high-alumina fly ash |
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|---|---|---|---|---|
| CN105274623A (en) * | 2015-10-27 | 2016-01-27 | 天津大学 | Method for in-situ growth of mullite whiskers by virtue of vacuum impregnation and freeze drying |
| CN105399401A (en) * | 2015-11-10 | 2016-03-16 | 太仓捷公精密金属材料有限公司 | Ceramic metal material |
| CN105347775A (en) * | 2015-12-08 | 2016-02-24 | 太原理工大学 | Preparation method of porous mullite ceramic applicable to diesel particulate filter |
| CN106278349A (en) * | 2016-08-10 | 2017-01-04 | 袁春华 | A kind of preparation method of low-density and high-strength polymer-coated ceramic powder proppant |
| CN106244135A (en) * | 2016-08-12 | 2016-12-21 | 郑州市少林滤材有限公司 | A kind of ceramsite propping agent compositions and its preparation method and application |
| CN106244135B (en) * | 2016-08-12 | 2018-12-28 | 郑州市少林滤材有限公司 | A kind of ceramsite propping agent composition and its preparation method and application |
| CN108854946A (en) * | 2018-06-07 | 2018-11-23 | 太原理工大学 | A kind of hierarchical porous structure zeolite absorption/catalyst and its construction method |
| CN108484201B (en) * | 2018-06-14 | 2020-07-31 | 哈尔滨工业大学 | Low-shrinkage porous silicon nitride ceramic and preparation method thereof |
| CN108484201A (en) * | 2018-06-14 | 2018-09-04 | 哈尔滨工业大学 | A kind of low-shrinkage porous silicon nitride ceramic and preparation method thereof |
| CN110903094A (en) * | 2019-12-25 | 2020-03-24 | 苏州纳迪微电子有限公司 | Spherical aluminum nitride and preparation method and application thereof |
| CN111559918A (en) * | 2020-05-27 | 2020-08-21 | 中国科学院上海硅酸盐研究所 | Method for preparing porous ceramic body by combining microemulsion with freeze drying |
| CN111559918B (en) * | 2020-05-27 | 2021-10-01 | 中国科学院上海硅酸盐研究所 | Method for preparing porous ceramic body by combining microemulsion with freeze drying |
| CN111763080A (en) * | 2020-06-22 | 2020-10-13 | 深圳市东有新材料科技有限公司 | Hollow mullite microspheres and preparation method thereof |
| CN111763080B (en) * | 2020-06-22 | 2022-08-30 | 深圳市东有新材料科技有限公司 | Hollow mullite microspheres and preparation method thereof |
| CN112811920A (en) * | 2021-02-09 | 2021-05-18 | 新沂北美高科耐火材料有限公司 | Ultrahigh-temperature refractory composite material and preparation method thereof |
| CN112811920B (en) * | 2021-02-09 | 2022-05-13 | 新沂北美高科耐火材料有限公司 | Ultrahigh-temperature refractory composite material and preparation method thereof |
| CN114572990A (en) * | 2022-03-15 | 2022-06-03 | 太原理工大学 | Preparation method of calcined kaolin with high oil absorption value |
| CN114853498A (en) * | 2022-04-22 | 2022-08-05 | 胜利油田新海兴达实业集团有限责任公司 | Micron ceramic ball material and preparation method and application thereof |
| CN115403364A (en) * | 2022-09-09 | 2022-11-29 | 天津大学 | Method for preparing columnar mullite by using rapid sintering process after pretreatment of high-alumina fly ash |
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