CN103436248B - Propping agent utilizing magnesium ore deposit mine tailing, iron ore mine, boric sludge standby and preparation method thereof - Google Patents
Propping agent utilizing magnesium ore deposit mine tailing, iron ore mine, boric sludge standby and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to propping agent.Its raw materials by weight of described propping agent comprises the component A of 80-90wt% and the B component of 10-20wt%; Wherein in component A containing magnesium ore deposit mine tailing, iron ore mine or ground silica and boron mud, or magnesium ore deposit mine tailing and iron ore mine or ground silica, or iron ore mine or ground silica and boron mud, B component is soft clay.The preparation method of described propping agent is: first magnesium ore deposit mine tailing is carried out light-burned process, then grinding; Magnesium ore deposit mine tailing after process is mixed with iron ore mine, boron mud and suppresses balling-up material, then by ball material mature calcined material and grinding: soft clay is carried out drying treatment, then grinding; Then raw material A is taken by proportioning and B mixes to obtain Preblend; By Preblend granulation, screening; Then send in rotary kiln, burn till, be incubated and obtain described propping agent.Propping agent of the present invention has high temperature resistant, high pressure resistant, corrosion-resistant, the feature such as high strength, high flow conductivity, low percentage of damage, and its preparation method energy consumption is little, and production capacity is large.
Description
Technical field
The present invention relates to fracturing propping agents and preparation method thereof, particularly relate to fracturing propping agents utilizing magnesium ore deposit mine tailing, iron ore mine, boric sludge standby and preparation method thereof.
Background technology
Pressure break refers in oil recovery or gas recovery, utilizes hydraulic action, makes hydrocarbon zone form a kind of method in crack.Hydrocarbon zone fracturing technology process fracturing truck, liquid high-pressure large-displacement with certain viscosity clamp-ons oil reservoir, after oil reservoir is extruded many cracks, add propping agent (as quartz sand etc.) filling and enter crack, improve the penetrating power of hydrocarbon zone, to increase water injection rate (water injection well) or oil offtake (oil well).Fracturing Technology plays an important role in the exploitation of oil, Sweet natural gas, and the effect of pressure break depends on the technical feature of fracturing propping agents largely.
After stratum presses off crack when propping agent is waterfrac treatment, be used for a kind of solid particulate that supporting crack do not make crack again closed.In use propping agent is mixed in fracturing liquid, utilizes high pressure tactics to inject deep layer rock fracture and support rock stratum, to improve Oil Guide rate, increase the object of crude production rate.Therefore propping agent is the critical material of pressing crack construction.For guaranteeing effectively strutting of underground deep layer pressure-break, suitable propping agent must be selected.
Sintering ceramsite, because intensity is high, degree of sphericity is good, is the fracturing propping agents of people's prioritizing selection.Traditional ceramsite propping agent is that by granulating powders, high temperature sintering forms, and the combination of finished product is high-strength corundum-mullite phase mutually, the propping agent disclosed in CN1085288A, CN101787270A with bauxitic clay and flint clay for raw material.But along with China's mine resources develops on a large scale, the main raw material bauxitic clay not only price increase amplitude that traditional method manufactures haydite is large, and bauxitic clay resource is also day by day nervous.Therefore, find cheap effectively alternative raw material production high-strength ceramic granule propping agent is one of pursuing a goal of this area always.
Forsterite-cordierite porcelain is when its crystalline phase comprises that forsterite accounts for 26-60%, trichroite accounts for 10-28%, enstatite accounts for 0.5-5%, the content of forsterite is greater than the content of trichroite, this porcelain has the advantages that thermal shock is stablized, physical strength is high, and experiment proves that the ceramsite propping agent utilizing this combination to produce mutually can meet the requirement of oil fracturing technique.Our country contains abundant wagnerite, boron stone, iron ore resource, but along with for many years continuous print exploitation has saved bit by bit a large amount of industrial tailings as boron mud, iron ore mine, magnesium ore deposit mine tailing etc., the discharge of these industrial tailings not only occupies a large amount of farmlands and mountain region, and become environmental pollution source, cause that mine resources reasonable utilization rate is low, the phenomenon of the vicious cycle such as development of resources expense is high.How utilizing the discarded industrial tailings such as boron mud, iron ore mine, magnesium ore deposit mine tailing to produce stay-in-grade ceramsite propping agent, is the work meant a great.
Summary of the invention
An object of the present invention is to provide a kind of low-density and high-strength ceramic proppant, propping agent provided by the present invention utilizes magnesium ore deposit mine tailing, iron ore mine or the industrial tailings such as ground silica, boron mud and soft clay to be raw material, burn till obtained by Raw material processing, granulating powders, high temperature, the combination of finished product is forsterite trichroite composite ceramics phase mutually, has high temperature resistant, high pressure resistant, corrosion-resistant, high strength, high flow conductivity, low percentage of damage, thermal shock resistance high.
One of propping agent provided by the present invention, its raw materials by weight comprises 80-90wt%, such as, be component A and the 10-20wt% of 81wt%, 84wt%, 88wt% etc., such as, be the B component of 11wt%, 14wt%, 17wt% etc.;
Wherein contain 30-55wt% in component A, be such as 32wt%, 34wt%, 38wt%, 42wt%, 46wt%, 49wt%, magnesium ore deposit mine tailing, the 20-35wt% of 53wt% etc., be such as the iron ore mine of 21wt%, 24wt%, 27wt%, 29wt%, 32wt%, 34wt% etc. or ground silica and 30 ~ 55wt%, be such as the boron mud of 32wt%, 34wt%, 38wt%, 42wt%, 44wt%, 48wt%, 52wt%, 54wt%, and component A can be magnesium ore deposit mine tailing, iron ore mine and boron mud, also can be magnesium ore deposit mine tailing, ground silica and boron mud, B component be soft clay;
Described propping agent adopts following method to prepare:
(1) magnesium ore deposit mine tailing is carried out light-burned process, through ball mill grinding;
(2) the magnesium ore deposit mine tailing after iron ore mine or ground silica, boron mud and step (1) ball milling is mixed, then suppress balling-up material;
(3) step (2) gained ball material is burnt till grog in rotary kiln, then through ball mill grinding;
(4) by after soft clay drying through ball mill grinding;
(5) soft clay after the grog after step (3) grinding and step (4) grinding is mixed in the ratio of described component A and B component obtain Preblend;
(6) by step (5) gained Preblend through the granulation of disk pelletizing machine, through screening obtain work in-process grain;
(7) step (6) gained work in-process grain is sent in rotary kiln, burn till, be incubated and obtain described propping agent;
Optionally carry out (8) by step (7) gained propping agent through bolting.Screening is the operation by the sieve of various different pore size, mixtures different for globule size being divided into various granularity level.Obtained propping agent product can be sieved into the propping agent of the different-grain diameters such as 20 ~ 40 orders, 30 ~ 50 orders, 40 ~ 70 orders through vibratory screening apparatus, the propping agent role of different-grain diameter is different, the performance evaluation of particle diameter on propping agent has very important impact, is one of selecting properly and the basis using propping agent.The weight percent sum of described raw material is 100%.
As optimal technical scheme, one of propping agent of the present invention, described component A contains the magnesium ore deposit mine tailing of 40-55wt%, the iron ore mine of 25-35wt% and the boron mud of 40 ~ 50wt%.The weight percent sum of described component is 100%.
Propping agent two provided by the invention, its raw materials by weight comprises 80-90wt%, such as, be component A and the 10-20wt% of 81wt%, 84wt%, 88wt% etc., such as, be the B component of 11wt%, 14wt%, 17wt% etc.;
Wherein contain 55-75wt% in component A, be such as magnesium ore deposit mine tailing and the 20-45wt% of 57wt%, 59wt%, 63wt%, 66wt%, 69wt%, 72wt%, 74wt% etc., be such as the iron ore mine of 21wt%, 24wt%, 27wt%, 29wt%, 32wt%, 34wt%, 38wt%, 42wt% etc., B component is soft clay;
Described propping agent adopts following method to prepare:
(1) magnesium ore deposit mine tailing is carried out light-burned process, through ball mill grinding;
(2) the magnesium ore deposit mine tailing after iron ore mine or ground silica and step (1) ball milling is mixed, then suppress balling-up material;
(3) step (2) gained ball material is burnt till grog in rotary kiln, then through ball mill grinding;
(4) by after soft clay drying through ball mill grinding;
(5) soft clay after the grog after step (3) grinding and step (4) grinding is mixed in the ratio of described component A and B component obtain Preblend;
(6) by step (5) gained Preblend through the granulation of disk pelletizing machine, through screening obtain work in-process grain;
(7) step (6) gained work in-process grain is sent in rotary kiln, burn till, be incubated and obtain described propping agent;
Optionally carry out (8) by step (7) gained propping agent through bolting.Screening is the operation by the sieve of various different pore size, mixtures different for globule size being divided into various granularity level.Obtained propping agent product can be sieved into the propping agent of the different-grain diameters such as 20 ~ 40 orders, 30 ~ 50 orders, 40 ~ 70 orders through vibratory screening apparatus, the propping agent role of different-grain diameter is different, the performance evaluation of particle diameter on propping agent has very important impact, is one of selecting properly and the basis using propping agent.The weight percent sum of described raw material is 100%.
As optimal technical scheme, propping agent two of the present invention, described component A contains the iron ore mine of 70-75wt% magnesium ore deposit mine tailing and 25-35wt%, preferably contains the iron ore mine of 75wt% magnesium ore deposit mine tailing and 25wt%.
Propping agent three provided by the present invention, its raw materials by weight comprises 80-90wt%, such as, be component A and the 10-20wt% of 81wt%, 84wt%, 88wt% etc., such as, be the B component of 11wt%, 14wt%, 17wt% etc.;
Wherein contain 10-30wt% in component A, be such as the iron ore mine of 11wt%, 14wt%, 17wt%, 21wt%, 24wt%, 27wt%, 29wt% etc. or the boron mud of ground silica and 70-90wt%, be such as 72wt%, 74wt%, 79wt%, 81wt%, 84wt%, 88wt% etc., B component is soft clay;
Described propping agent adopts following method to prepare:
(1) iron ore mine or ground silica and boron mud are mixed, then suppress balling-up material;
(2) step (1) gained ball material is burnt till grog in rotary kiln, then through ball mill grinding;
(3) by after soft clay drying through ball mill grinding;
(4) soft clay after the grog after step (2) grinding and step (3) grinding is mixed in the ratio of described component A and B component obtain Preblend;
(5) by step (4) gained Preblend through the granulation of disk pelletizing machine, through screening obtain work in-process grain;
(6) step (5) gained work in-process grain is sent in rotary kiln, burn till, be incubated and obtain described propping agent;
Optionally carry out (7) by step (8) gained propping agent through bolting.
As optimal technical scheme, one of propping agent of the present invention and the boron mud described in three be borax produce in produce waste residue.The color of described boron mud is light brown, belongs to not easily soluble substance, the stickiness that tool is certain, and plasticity-is better, relative density 2.3g/cm
3, tap density 1.8g/cm
3, about particle diameter 150 order, the new boron mud produced includes the free-water of about 30%.Boron mud is in alkalescence, and pH value is 8 ~ 10.Containing alkaline matters such as magnesium oxide, calcium oxide, sodium oxides in boron mud.Boron part that mud discharges, not even a blade of grass grows, and its alkali lye can be added in underground water, makes the farmland underproduction of surrounding, and severe patient can make farm crop have no harvest, and produce pollution to the tap water of surrounding.Because boron mud particle is comparatively thin, after drying out, usually can disperse with the wind, atmospheric environment be produced and pollutes.Boron mud has become a kind of public hazards to the pollution of ecotope, the pollution of atmospheric environment.Therefore, boron mud is used in the preparation of propping agent by the present invention, on the one hand refuse is fully used, improves environment, has also obtained the propping agent having economic worth on the other hand.
As optimal technical scheme, propping agent of the present invention, its raw materials by weight comprises the component A of 83wt% and the B component of 17wt%.
As optimal technical scheme, propping agent of the present invention, described magnesium ore deposit mine tailing is that magnesium ore deposit is except superfine magnesite, one-level magnesite, the mine tailing not comprising calcium block outside secondary magnesite or three grades of magnesites or at least 2 persons, such as not comprising the mine tailing of calcium block except superfine magnesite or secondary magnesite or three grades of magnesites, or for not comprising the mine tailing of calcium block except superfine magnesite and secondary magnesite, or for removing superfine magnesite, the mine tailing of calcium block is not comprised outside one-level magnesite and secondary magnesite, or for removing superfine magnesite, one-level magnesite, the mine tailing of calcium block is not comprised outside secondary magnesite and three grades of magnesites, be preferably In Dashiqiao Area, Yingkou magnesite except superfine magnesite, one-level magnesite, the mine tailing not comprising calcium block outside secondary magnesite or three grades of magnesites or at least 2 persons.
Preferably, described iron ore mine is the mine tailing after iron ore removing iron ore concentrate, is preferably the mine tailing of iron ore after magnetic separation, flotation removing iron ore concentrate.
Preferably, described ground silica is the 120-200 order ground silica that dioxide-containing silica is greater than 97%.This ground silica can form through water mill.
Preferably, described soft clay is ball clay, is preferably the ball clay of more than three grades, the more preferably ball clay of Jilin Cortex Fraxini mandshuricae more than three grades.
Due to the overexploitation of boron rock, iron ore, magnesium ore resources, resource recoverable amount wretched insufficiency, mine tailing serious waste.Therefore the mine tailing utilizing boron rock, iron ore, magnesium ore deposit more effectively, fully provided by the present invention, has administered mine tailing, has improve resource utilization.
The present invention utilizes the discarded industrial tailings such as magnesium ore deposit tailing, boron mud, iron ore mine to be prepared propping agent, day by day expensive bauxitic clay resource can be substituted, particularly suitable purposes can be searched out in In Dashiqiao Area, Yingkou again for discarded industrial tailings, improve the industrial chain of magnesium ore deposit, boron rock, iron ore, more valuable is a kind of method finding very actual improvement industrial tailings.
An object of the present invention is also the preparation method providing described propping agent, and described method comprises the steps:
(1) magnesium ore deposit mine tailing is carried out light-burned process, through ball mill grinding;
(2) by the magnesium ore deposit mine tailing after iron ore mine or ground silica, boron mud and step (1) ball milling by one of propping agent provided by the invention or two or three (this combination is not due to containing magnesium ore deposit mine tailing, step (1) can be omitted) desired raw material, required ratio mix, and then suppresses balling-up material;
(3) step (2) gained ball material is burnt till grog in rotary kiln, then through ball mill grinding;
(4) by after soft clay drying through ball mill grinding;
(5) soft clay after the grog after step (3) grinding and step (4) grinding is mixed in the ratio of component A of the present invention and B component obtain Preblend;
(6) by step (5) gained Preblend through the granulation of disk pelletizing machine, through screening obtain work in-process grain;
(7) step (6) gained work in-process grain is sent in rotary kiln, burn till, be incubated and obtain described propping agent;
Optionally carry out (8) by step (7) gained propping agent through bolting.
Preferably, the calcining temperature of the light-burned process described in step (1) is more than 1000 DEG C, such as, be 1020 DEG C, 1070 DEG C, 1110 DEG C, 1150 DEG C, 1170 DEG C, 1190 DEG C, 1200 DEG C, 1230 DEG C etc., preferably 1100 ~ 1250 DEG C; Light-burned is roasting refractory raw material at a lower temperature, makes it complete a part of physical-chemical reaction and a kind of processing method that raw material is activated.Fixed material is had to the light roasting temperature an of the best.The too high meeting of light roasting temperature makes crystallization degree increase, and granularity becomes large, and specific surface area and activity decrease, light roasting temperature is too low, may have residual undecomposed female salt and hinder sintering.
Preferably, the granularity of described grinding is more than 120 orders, such as, be 140 orders, 170 orders, 230 orders, 270 orders etc., is preferably 120-200 order, more preferably 120 orders.
Preferably, mixing described in step (2) adopts forced stirrer to carry out;
Preferably, described compacting adopts ball press to carry out;
Preferably, the temperature of burning till described in step (3) is 1000-1300 DEG C, such as, be 1030 DEG C, 1060 DEG C, 1150 DEG C, 1190 DEG C, 1210 DEG C, 1240 DEG C, 1270 DEG C, 1300 DEG C etc., is preferably 1200-1250 DEG C;
Preferably, described in time of burning till be more than 0.5h, be such as 0.7h, 0.9h, 1.2h, 1.4h, 1.6h, 2.0h, 2.4h, 2.8h, 3.2h etc., be preferably 0.5-2h, more preferably 1.5h;
Preferably, the granularity of described grinding is more than 600 orders, such as, be 650 orders, 750 orders, 800 orders etc., is preferably 600-700 order, more preferably 600 orders.
Preferably, temperature dry described in step (4) is more than 300 DEG C, such as, be 320 DEG C, 340 DEG C, 370 DEG C, 395 DEG C, 420 DEG C, 440 DEG C, 480 DEG C, 510 DEG C etc., be preferably more than 350 DEG C, more preferably 350-450 DEG C;
Preferably, the granularity of described grinding is more than 500 orders, such as, be 540 orders, 650 orders, 800 orders etc., is preferably 600-700 order, more preferably 600 orders;
Preferably, described in step (6), the granularity of work in-process grain is 12-70 order;
Preferably, the temperature of burning till described in step (7) is more than 1000 DEG C, such as, be 1030 DEG C, 1060 DEG C, 1150 DEG C, 1190 DEG C, 1210 DEG C, 1240 DEG C, 1270 DEG C, 1300 DEG C etc., is preferably 1210 ~ 1280 DEG C;
Preferably, described soaking time is more than 1h, such as, be 1.2h, 1.4h, 1.6h, 2.0h, 2.4h, 2.8h, 3.2h etc., is preferably 1.5 ~ 2.5h.
The industrial tailings that the present invention utilizes magnesium ore deposit mine tailing, iron ore mine, boron mud etc. discarded, introduce the soft clay that the binding ability of some is strong, by processing technology routine of the present invention, the ceramsite propping agent that intensity is high, thermal shock resistance is stable forsterite trichroite composite ceramics combines can be synthesized.
The present invention has following actively useful effect:
1. ceramic product smooth surface of the present invention, densification, has that compressive strength is high, volume density is low, chemical stability and a good excellent properties of acid resistance, and the one-tenth of product is grouped in table 1, and relevant performance index refer to table 2.
2. ceramic product main raw material of the present invention is magnesium ore deposit mine tailing, iron ore mine, boron mud, makes the best use of everything, and exquisiteness of drawing materials is with low cost, wide material sources.More rare is administered mine tailing, has transformed environment, helps bargh to reduce the expense of tailings discharging, extends the life-span in mine, improve the utilising efficiency of resource.
3. the raw materials for production that the present invention changes current haydite use high bauxitic clay resource, change corundum-mullite in conjunction with phase, adopt the waste resources such as magnesium ore deposit mine tailing, iron ore mine, boron mud, use soft clay to make its synthetic forsterite trichroite composite ceramics phase.This crystalline phase has high temperature resistant, high pressure resistant, that heat-resistant knocking stability is excellent feature, and therefore product of the present invention has excellent use properties.
4. and preparation technology's energy consumption of the present invention little, production capacity is large.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.
Embodiment one
A kind of propping agent, raw materials is configured to: first produce synthetic material in following ratio: magnesium ore deposit mine tailing 45wt%, iron ore mine 25wt% and boron mud 30wt%, get synthetic material 83wt% and soft clay 17wt%.
The preparation method of above-mentioned high-strength ceramic granule propping agent, comprises the steps:
(1) magnesium ore deposit mine tailing is carried out light-burned process through the calcining temperature of 1100 DEG C, then through ball mill grinding to 200 order;
(2) the magnesium ore deposit mine tailing 200 order powder of (1) milled, iron ore mine and boron mud are suppressed balling-up through ball press in proportion after forced stirrer mixes;
(3) by the grog of the ball material pressed gained after rotary kiln 1200 DEG C × 1h burns till through ball mill grinding 600 order; Soft clay through 400 DEG C of drying treatment, more respectively through ball mill grinding 600 order;
(4) raw material after step (3) process is made into compound in proportion, and mixes to obtain Preblend;
(5) by the Preblend mixed of step (4) gained through the granulation of disk pelletizing machine, through screening obtain work in-process grain 12-70 order;
(6) sent in rotary kiln by the work in-process grain of step (5) gained, burn till at 1260 DEG C, namely insulation 1h obtains described propping agent;
(7) high temperature of step (6) gained is burnt till haydite through bolting, obtain the propping agent of different size; Final product after screening is through packing warehouse-in after the assay was approved.
Embodiment two
A kind of propping agent, raw materials is configured to: first produce synthetic material in following ratio: magnesium ore deposit mine tailing 30wt%, ground silica 30wt% and boron mud 40wt%, get synthetic material 90wt% and soft clay 10wt%.
The preparation method of above-mentioned high-strength ceramic granule propping agent, comprises the steps:
(1) magnesium ore deposit mine tailing is carried out light-burned process through the calcining temperature of 1140 DEG C, then through ball mill grinding to 140 order;
(2) the magnesium ore deposit mine tailing 140 order powder of (1) milled, iron ore mine and boron mud are suppressed balling-up through ball press in proportion after forced stirrer mixes;
(3) by the grog of the ball material pressed gained after rotary kiln 1250 DEG C × 1.5h burns till through ball mill grinding 600 order; Soft clay through 400 DEG C of drying treatment, more respectively through ball mill grinding 600 order;
(4) raw material after step (3) process is made into compound in proportion, and mixes to obtain Preblend;
(5) by the Preblend mixed of step (4) gained through the granulation of disk pelletizing machine, through screening obtain work in-process grain 12-70 order;
(6) sent in rotary kiln by the work in-process grain of step (5) gained, burn till at 1220 DEG C, namely insulation 1.5h obtains described propping agent;
(7) high temperature of step (6) gained is burnt till haydite through bolting, obtain the propping agent of different size; Final product after screening is through packing warehouse-in after the assay was approved.
Embodiment three
A kind of propping agent, raw materials is configured to: first produce synthetic material in following ratio: magnesium ore deposit mine tailing 40wt%, iron ore mine 20wt% and boron mud 40wt%, get synthetic material 83%wt and soft clay 17wt%.
The preparation method of above-mentioned high-strength ceramic granule propping agent, comprises the steps:
(1) magnesium ore deposit mine tailing is carried out light-burned process through the calcining temperature of 1250 DEG C, then through ball mill grinding to 180 order;
(2) the magnesium ore deposit tail 180 order powder of (1) milled, iron ore mine and boron mud are suppressed balling-up through ball press in proportion after forced stirrer mixes;
(3) by the grog of the ball material pressed gained after rotary kiln 1250 DEG C × 0.5h burns till through ball mill grinding 600 order; Soft clay through 350 DEG C of drying treatment, more respectively through ball mill grinding 600 order;
(4) raw material after step (3) process is made into compound in proportion, and mixes to obtain Preblend;
(5) by the Preblend mixed of step (4) gained through the granulation of disk pelletizing machine, through screening obtain work in-process grain 12-70 order;
(6) sent in rotary kiln by the work in-process grain of step (5) gained, 1280 DEG C are burnt till, and namely insulation 2h obtains described propping agent.
Embodiment four
A kind of propping agent, raw materials is configured to: first produce synthetic material in following ratio: magnesium ore deposit mine tailing 35wt%, ground silica 25wt% and boron mud 40wt%, get synthetic material 85wt% and soft clay 15wt%.
The preparation method of above-mentioned high-strength ceramic granule propping agent, comprises the steps:
(1) magnesium ore deposit mine tailing is carried out light-burned process through the calcining temperature of 1100 DEG C, then through ball mill grinding to 120 order;
(2) the magnesium ore deposit mine tailing 120 order powder of (1) milled, iron ore mine and boron mud are suppressed balling-up through ball press in proportion after forced stirrer mixes;
(3) by the grog of the ball material pressed gained after rotary kiln 1250 DEG C × 1.5h burns till through ball mill grinding 600 order; Soft clay through 400 DEG C of drying treatment, more respectively through ball mill grinding 600 order;
(4) raw material after step (3) process is made into compound in proportion, and mixes to obtain Preblend;
(5) by the Preblend mixed of step (4) gained through the granulation of disk pelletizing machine, through screening obtain work in-process grain 12-70 order;
(6) sent in rotary kiln by the work in-process grain of step (5) gained, 1260 DEG C are burnt till, and namely insulation 2.0h obtains described propping agent;
(7) high temperature of step (6) gained is burnt till haydite through bolting, obtain the propping agent of different size; Final product after screening is through packing warehouse-in after the assay was approved.
Embodiment five
A kind of propping agent, raw materials is configured to: first produce synthetic material in following ratio: iron ore mine 20wt% and boron mud 80wt%, get synthetic material 83wt% and soft clay 17wt%.
The preparation method of above-mentioned high-strength ceramic granule propping agent, comprises the steps:
(1) iron ore mine and boron mud are suppressed balling-up through ball press in proportion after forced stirrer mixes;
(2) by the grog of the ball material pressed gained after rotary kiln 1200 DEG C × 1.0h burns till through ball mill grinding 600 order; Soft clay through 350 DEG C of drying treatment, more respectively through ball mill grinding 600 order;
(3) raw material after step (2) process is made into compound in proportion, and mixes to obtain Preblend;
(4) by the Preblend mixed of step (3) gained through the granulation of disk pelletizing machine, through screening obtain work in-process grain 12-70 order;
(5) sent in rotary kiln by the work in-process grain of step (4) gained, 1260 DEG C are burnt till, and namely insulation 2h obtains described propping agent;
(6) high temperature of step (5) gained is burnt till haydite through bolting, obtain the propping agent of different size; Final product after screening is through packing warehouse-in after the assay was approved.
Embodiment six
A kind of propping agent, raw materials is configured to: first produce synthetic material in following ratio: magnesium ore deposit mine tailing 70wt%, iron ore mine 30wt%, get synthetic material 83wt% and soft clay 17wt%.
The preparation method of above-mentioned high-strength ceramic granule propping agent, comprises the steps:
(1) magnesium ore deposit mine tailing is carried out light-burned process through the calcining temperature of 1100 DEG C, then through ball mill grinding to 210 order;
(2) the magnesium ore deposit mine tailing 210 order powder of (1) milled, iron ore mine are suppressed balling-up through ball press in proportion after forced stirrer mixes;
(3) by the grog of the ball material pressed gained after rotary kiln 1200 DEG C × 1h burns till through ball mill grinding 600 order; Soft clay through 400 DEG C of drying treatment, more respectively through ball mill grinding 600 order;
(4) raw material after step (3) process is made into compound in proportion, and mixes to obtain Preblend;
(5) by the Preblend mixed of step (4) gained through the granulation of disk pelletizing machine, through screening obtain work in-process grain 12-70 order;
(6) sent in rotary kiln by the work in-process grain of step (5) gained, burn till at 1210 DEG C, namely insulation 2h obtains described propping agent;
(7) high temperature of step (6) gained is burnt till haydite through bolting, obtain the propping agent of different size; Final product after screening is through packing warehouse-in after the assay was approved.
Embodiment seven
A kind of propping agent, raw materials is configured to: first produce synthetic material in following ratio: magnesium ore deposit mine tailing 75wt%, ground silica 25wt%, get synthetic material 85wt% and soft clay 15wt%.
The preparation method of above-mentioned high-strength ceramic granule propping agent, comprises the steps:
(1) magnesium ore deposit mine tailing is carried out light-burned process through the calcining temperature of 1000 DEG C, then through ball mill grinding to 230 order;
(2) the magnesium ore deposit mine tailing 230 order powder of (1) milled, iron ore mine are suppressed balling-up through ball press in proportion after forced stirrer mixes;
(3) by the grog of the ball material pressed gained after rotary kiln 1250 DEG C × 1.5h burns till through ball mill grinding 700 order; Soft clay through 350 DEG C of drying treatment, more respectively through ball mill grinding 600 order;
(4) raw material after step (3) process is made into compound in proportion, and mixes to obtain Preblend;
(5) by the Preblend mixed of step (4) gained through the granulation of disk pelletizing machine, through screening obtain work in-process grain 12-70 order;
(6) sent in rotary kiln by the work in-process grain of step (5) gained, 1260 DEG C are burnt till, and namely insulation 2.0h obtains described propping agent.
Haydite made by embodiment one to embodiment seven is carried out component content test, the results are shown in Table 1, and performance test, the results are shown in Table 2.
Table 1
| Composition | wt% |
| SiO 2 | 50～58 |
| Al 2O 3 | 7～12 |
| MgO | 25～33 |
| Fe 2O 3 | 1～5.5 |
| Other | 0～2.5% |
Table 2
| Project | Index |
| Specification (mm) | 0.425～0.85 |
| Percentage of damage (69Mpa) | ≤15% |
| Volume density (g/cm 3） | ≤1.6 |
| Volume density (g/cm 3） | ≤2.76 |
| Circularity | ≥0.9 |
| Sphericity | ≥0.9 |
| Acid solubility (%) | ≤7 |
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (23)
1. a preparation method for propping agent, is characterized in that, described propping agent raw materials by weight is made up of the component A of 80-90wt% and the B component of 10-20wt%;
Wherein component A is made up of the magnesium ore deposit mine tailing of 30-55wt%, the iron ore mine of 20-35wt% or the boron mud of ground silica and 30 ~ 55wt%, and above-mentioned each component sum is 100%, and B component is soft clay;
Described proppant production method is as follows:
(1) magnesium ore deposit mine tailing is carried out light-burned process, through ball mill grinding;
(2) the magnesium ore deposit mine tailing after iron ore mine or ground silica, boron mud and step (1) ball milling is mixed, then suppress balling-up material;
(3) step (2) gained ball material is burnt till grog in rotary kiln, then through ball mill grinding;
(4) by after soft clay drying through ball mill grinding;
(5) soft clay after the grog after step (3) grinding and step (4) grinding is mixed in the ratio of described component A and B component obtain Preblend;
(6) by step (5) gained Preblend through the granulation of disk pelletizing machine, through screening obtain work in-process grain;
(7) step (6) gained work in-process grain is sent in rotary kiln, burn till, be incubated and obtain described propping agent;
Optionally carry out (8) by step (7) gained propping agent through bolting;
The calcining temperature of the light-burned process described in step (1) is more than 1000 DEG C; The granularity of described grinding is more than 120 orders;
Mixing described in step (2) adopts forced stirrer to carry out; Described compacting adopts ball press to carry out;
The temperature of burning till described in step (3) is 1000-1300 DEG C; The described time of burning till is 0.5-2h; The granularity of described grinding is more than 600 orders;
Temperature dry described in step (4) is more than 300 DEG C; The granularity of described grinding is more than 500 orders;
Described in step (6), the granularity of work in-process grain is 12-70 order;
The temperature of burning till described in step (7) is more than 1000 DEG C; Described soaking time is 1.5 ~ 2.5h.
2. a preparation method for propping agent, is characterized in that, described propping agent raw materials by weight is made up of the component A of 80-90wt% and the B component of 10-20wt%;
Wherein be made up of the magnesium ore deposit mine tailing of 55-75wt% and the iron ore mine of 20-45wt% or ground silica in component A, above-mentioned each component sum is 100%, and B component is soft clay;
Described proppant production method is as follows:
(1) magnesium ore deposit mine tailing is carried out light-burned process, through ball mill grinding;
(2) the magnesium ore deposit mine tailing after iron ore mine or ground silica and step (1) ball milling is mixed, then suppress balling-up material;
(3) step (2) gained ball material is burnt till grog in rotary kiln, then through ball mill grinding;
(4) by after soft clay drying through ball mill grinding;
(5) soft clay after the grog after step (3) grinding and step (4) grinding is mixed in the ratio of described component A and B component obtain Preblend;
(6) by step (5) gained Preblend through the granulation of disk pelletizing machine, through screening obtain work in-process grain;
(7) step (6) gained work in-process grain is sent in rotary kiln, burn till, be incubated and obtain described propping agent;
Optionally carry out (8) by step (7) gained propping agent through bolting;
The calcining temperature of the light-burned process described in step (1) is more than 1000 DEG C; The granularity of described grinding is more than 120 orders;
Mixing described in step (2) adopts forced stirrer to carry out; Described compacting adopts ball press to carry out;
The temperature of burning till described in step (3) is 1000-1300 DEG C; The described time of burning till is 0.5-2h; The granularity of described grinding is more than 600 orders;
Temperature dry described in step (4) is more than 300 DEG C; The granularity of described grinding is more than 500 orders;
Described in step (6), the granularity of work in-process grain is 12-70 order;
The temperature of burning till described in step (7) is more than 1000 DEG C; Described soaking time is 1.5 ~ 2.5h.
3. a preparation method for propping agent, is characterized in that, described propping agent raw materials by weight is made up of the component A of 80-90wt% and the B component of 10-20wt%;
Wherein component A is made up of the iron ore mine of 10-30wt% or the boron mud of ground silica and 70-90wt%, and B component is soft clay;
Described proppant production method is as follows:
(1) iron ore mine or ground silica and boron mud are mixed, then suppress balling-up material;
(2) step (1) gained ball material is burnt till grog in rotary kiln, then through ball mill grinding;
(3) by after soft clay drying through ball mill grinding;
(4) soft clay after the grog after step (2) grinding and step (3) grinding is mixed in the ratio of described component A and B component obtain Preblend;
(5) by step (4) gained Preblend through the granulation of disk pelletizing machine, through screening obtain work in-process grain;
(6) step (5) gained work in-process grain is sent in rotary kiln, burn till, be incubated and obtain described propping agent;
Optionally carry out (7) by step (8) gained propping agent through bolting;
The calcining temperature of the light-burned process described in step (1) is more than 1000 DEG C; The granularity of described grinding is more than 120 orders;
Mixing described in step (2) adopts forced stirrer to carry out; Described compacting adopts ball press to carry out;
The temperature of burning till described in step (3) is 1000-1300 DEG C; The described time of burning till is 0.5-2h; The granularity of described grinding is more than 600 orders;
Temperature dry described in step (4) is more than 300 DEG C; The granularity of described grinding is more than 500 orders;
Described in step (6), the granularity of work in-process grain is 12-70 order;
The temperature of burning till described in step (7) is more than 1000 DEG C; Described soaking time is 1.5 ~ 2.5h.
4. the preparation method of the propping agent according to any one of claim 1-3, is characterized in that, its raw materials by weight is made up of the component A of 83wt% and the B component of 17wt%.
5. the preparation method of propping agent according to claim 2, is characterized in that, described component A is made up of the iron ore mine of 70-75wt% magnesium ore deposit mine tailing and 25-35wt% or ground silica, and above-mentioned each component sum is 100%.
6. the preparation method of propping agent according to claim 5, is characterized in that, described component A is made up of the iron ore mine of 75wt% magnesium ore deposit mine tailing and 25wt% or ground silica.
7. the preparation method of the propping agent according to claim 1 or 3, is characterized in that, described boron mud is the waste residue produced during borax is produced.
8. the preparation method of the propping agent according to any one of claim 1-3, is characterized in that, described magnesium ore deposit mine tailing is the mine tailing that do not comprise calcium block of magnesium ore deposit except superfine magnesite, one-level magnesite, secondary magnesite or three grades of magnesites or at least 2 persons.
9. the preparation method of propping agent according to claim 8, is characterized in that, described magnesium ore deposit mine tailing is the mine tailing that do not comprise calcium block of In Dashiqiao Area, Yingkou magnesite except superfine magnesite, one-level magnesite, secondary magnesite or three grades of magnesites or at least 2 persons.
10. the preparation method of the propping agent according to any one of claim 1-3, is characterized in that, described iron ore mine is the mine tailing after iron ore removing iron ore concentrate.
The preparation method of 11. propping agents according to claim 10, is characterized in that, described iron ore mine is the mine tailing of iron ore after magnetic separation, flotation removing iron ore concentrate.
The preparation method of 12. propping agents according to any one of claim 1-3, it is characterized in that, described ground silica is the 120-200 order ground silica that dioxide-containing silica is greater than 97%.
The preparation method of 13. propping agents according to any one of claim 1-3, it is characterized in that, described soft clay is ball clay.
The preparation method of 14. propping agents according to claim 13, is characterized in that, described soft clay is the ball clay of more than three grades.
The preparation method of 15. propping agents according to claim 14, is characterized in that, described soft clay is the ball clay of Jilin Cortex Fraxini mandshuricae more than three grades.
16. preparation methods according to any one of claim 1-3, it is characterized in that, the calcining temperature of the light-burned process described in step (1) is 1100 ~ 1250 DEG C.
17. preparation methods according to any one of claim 1-3, it is characterized in that, described in step (1), the granularity of grinding is 120-200 order.
18. preparation methods according to any one of claim 1-3, it is characterized in that, the temperature of burning till described in step (3) is 1200-1250 DEG C.
19. preparation methods according to any one of claim 1-3, it is characterized in that, the time of burning till described in step (3) is 1.5h.
20. preparation methods according to any one of claim 1-3, it is characterized in that, described in step (3), the granularity of grinding is 600-700 order.
21. preparation methods according to any one of claim 1-3, is characterized in that, temperature dry described in step (4) is more than 350 DEG C.
22. preparation methods according to any one of claim 1-3, it is characterized in that, described in step (4), the granularity of grinding is 600-700 order.
23. preparation methods according to any one of claim 1-3, it is characterized in that, the temperature of burning till described in step (7) is 1210 ~ 1280 DEG C.
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| CN103725281B (en) * | 2013-12-24 | 2015-06-17 | 营口腾隆新材料有限公司 | Preparation method of low-cost petroleum fracturing propping agent |
| CN105399434A (en) * | 2015-12-04 | 2016-03-16 | 刘冬学 | Boric sludge ceramsite and preparation method thereof |
| RU2694363C1 (en) * | 2016-02-19 | 2019-07-12 | Общество С Ограниченной Ответственностью "Ника-Петротэк" | Ceramic proppant and its production method |
| CN108718993B (en) * | 2018-07-13 | 2020-06-26 | 大连地拓环境科技有限公司 | Boron tailing planting soil and preparation method thereof |
| CN117985967B (en) * | 2024-02-05 | 2024-10-22 | 河南理工大学 | Magnesium tailing admixture and preparation method and application thereof |
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| WO2008094069A2 (en) * | 2006-12-27 | 2008-08-07 | Schlumberger Canada Limited | Proppant, proppant production method and use of proppant |
| WO2012151091A1 (en) * | 2011-05-05 | 2012-11-08 | Basf Se | A proppant |
| CN103173203A (en) * | 2013-03-29 | 2013-06-26 | 杨松 | Proppant prepared by utilizing industrial tailings and preparation method thereof |
| CN103193461A (en) * | 2013-03-29 | 2013-07-10 | 杨松 | Proppant prepared from tailings of magnesium ore, boron ore and iron ore and preparation method thereof |
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| WO2008094069A2 (en) * | 2006-12-27 | 2008-08-07 | Schlumberger Canada Limited | Proppant, proppant production method and use of proppant |
| WO2012151091A1 (en) * | 2011-05-05 | 2012-11-08 | Basf Se | A proppant |
| CN103173203A (en) * | 2013-03-29 | 2013-06-26 | 杨松 | Proppant prepared by utilizing industrial tailings and preparation method thereof |
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