CN113582676A - Magnesium aluminum silicate proppant and production process and application thereof - Google Patents
Magnesium aluminum silicate proppant and production process and application thereof Download PDFInfo
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- CN113582676A CN113582676A CN202111017216.5A CN202111017216A CN113582676A CN 113582676 A CN113582676 A CN 113582676A CN 202111017216 A CN202111017216 A CN 202111017216A CN 113582676 A CN113582676 A CN 113582676A
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- aluminum silicate
- magnesium aluminum
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- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 190
- 239000002994 raw material Substances 0.000 claims abstract description 70
- 239000000463 material Substances 0.000 claims abstract description 51
- 238000001035 drying Methods 0.000 claims abstract description 44
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims abstract description 33
- 239000004615 ingredient Substances 0.000 claims abstract description 20
- 239000011435 rock Substances 0.000 claims abstract description 18
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 16
- 239000011707 mineral Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 35
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000005469 granulation Methods 0.000 claims description 22
- 230000003179 granulation Effects 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 22
- 239000011230 binding agent Substances 0.000 claims description 18
- 238000007493 shaping process Methods 0.000 claims description 18
- 239000000292 calcium oxide Substances 0.000 claims description 16
- 235000012255 calcium oxide Nutrition 0.000 claims description 16
- 235000010755 mineral Nutrition 0.000 claims description 15
- 239000010450 olivine Substances 0.000 claims description 11
- 229910052609 olivine Inorganic materials 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052681 coesite Inorganic materials 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 229910052682 stishovite Inorganic materials 0.000 claims description 10
- 229910052905 tridymite Inorganic materials 0.000 claims description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 7
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 6
- 239000003245 coal Substances 0.000 claims description 6
- 229910052900 illite Inorganic materials 0.000 claims description 6
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- 229910052620 chrysotile Inorganic materials 0.000 claims description 4
- 239000010881 fly ash Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- CWBIFDGMOSWLRQ-UHFFFAOYSA-N trimagnesium;hydroxy(trioxido)silane;hydrate Chemical compound O.[Mg+2].[Mg+2].[Mg+2].O[Si]([O-])([O-])[O-].O[Si]([O-])([O-])[O-] CWBIFDGMOSWLRQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910010272 inorganic material Inorganic materials 0.000 claims description 3
- 239000011147 inorganic material Substances 0.000 claims description 3
- 238000005550 wet granulation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 239000002910 solid waste Substances 0.000 abstract description 5
- 239000003208 petroleum Substances 0.000 abstract description 4
- 239000010878 waste rock Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 17
- 238000010438 heat treatment Methods 0.000 description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 230000008901 benefit Effects 0.000 description 8
- 239000006004 Quartz sand Substances 0.000 description 7
- 229940009868 aluminum magnesium silicate Drugs 0.000 description 7
- WMGSQTMJHBYJMQ-UHFFFAOYSA-N aluminum;magnesium;silicate Chemical compound [Mg+2].[Al+3].[O-][Si]([O-])([O-])[O-] WMGSQTMJHBYJMQ-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000007613 environmental effect Effects 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- 238000001354 calcination Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000003345 natural gas Substances 0.000 description 5
- 239000011246 composite particle Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 239000003209 petroleum derivative Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000010883 coal ash Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 2
- 239000000391 magnesium silicate Substances 0.000 description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 description 2
- 235000019792 magnesium silicate Nutrition 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
本发明提供了一种硅酸镁铝支撑剂及其生产工艺和应用。生产工艺包括：将含蛇纹石矿物的原料进行干燥和破碎，获得原料粉体；将原料粉体进行焙烧，得到硅酸镁铝粉体；将硅酸镁铝粉体与配料进行混合，获得混合物料粉体；将混合物料粉体进行造粒，获得球形颗粒状坯体；将球形颗粒状坯体进行干燥和烧结，获得硅酸镁铝支撑剂。根据本发明，可以以主要含蛇纹石的岩石、废石、尾矿为原料生产高强度低密度石油压裂硅酸镁铝支撑剂，实现了多种固体废物的资源化利用。
The invention provides a magnesium aluminum silicate proppant and its production process and application. The production process includes: drying and crushing the raw material containing serpentine minerals to obtain raw material powder; roasting the raw material powder to obtain magnesium aluminum silicate powder; mixing the magnesium aluminum silicate powder with ingredients to obtain Mixing material powder; granulating the mixed material powder to obtain a spherical granular blank; drying and sintering the spherical granular blank to obtain a magnesium aluminum silicate proppant. According to the present invention, high-strength and low-density magnesium-aluminum silicate proppant for petroleum fracturing can be produced by using mainly serpentine-containing rock, waste rock, and tailings as raw materials, thereby realizing the resource utilization of various solid wastes.
Description
Technical Field
The invention belongs to the field of oil and gas application materials, and particularly relates to a production process of a magnesium aluminum silicate proppant, a magnesium aluminum silicate proppant product obtained by the process and application of the magnesium aluminum silicate proppant product.
Background
When the petroleum and natural gas deep well is exploited, in order to crack the petroleum and natural gas containing rock stratum, the petroleum and natural gas are collected from a channel formed by the crack, a petroleum propping agent enters the stratum along with a high-pressure solution and is filled in the crack of the rock stratum, so that the pressure exceeding the fracture strength of the stratum enables the rock stratum around a shaft to generate the crack, and the oil and gas products can smoothly pass through the crack, thereby increasing the yield.
Petroleum proppants need to meet the following requirements: (1) the artificial crack has enough compressive strength and abrasion resistance, can bear strong pressure and friction force during injection, and effectively supports the artificial crack; (2) the proppant particles have low relative density and are convenient to pump into the well; (3) under the condition that the temperature is 200 ℃, the proppant particles do not have chemical action with fracturing fluid and reservoir fluid, and the acid solubility is less than 7%.
Because of the difference of oil layer depth, grease viscosity, the requirement of different oil fields to proppant is also different, there are four kinds of proppant of high strength high density, high strength medium density and high strength low density and high strength ultra low density in the existing market, the mesh number commonly used has: 16-30 meshes, 20-40 meshes, 30-50 meshes, 40-70 meshes and the like.
The conventional proppant mainly comprises quartz sand, bauxite ceramsite sand, resin-coated composite particles and the like. The quartz sand is low in cost, low in density and easy to pump, occupies more than 50% of the market share of the proppant at present, but is low in strength and poor in sphericity, and is not suitable for deep wells with high closing pressure. Although the sphericity of the composite particles of the resin-coated quartz sand is improved, the composite particles have strong corrosion resistance and good flow conductivity, the composite particles are difficult to push due to short product retention period and high manufacturing cost.
The oil fracturing propping agent is an essential auxiliary material in the oil and gas field exploitation process, has important effects on improving oil yield, natural gas yield and the like, and at present, many propping agents have the defects of low strength, large density, high manufacturing cost and the like.
Disclosure of Invention
The present invention aims to address at least one of the above-mentioned deficiencies of the prior art. For example, one of the objects of the present invention is to provide a process for producing a proppant of magnesium aluminum silicate. As another example, another object of the present invention is to provide a magnesium aluminum silicate proppant.
In order to achieve the above object, an aspect of the present invention provides a production process of a magnesium aluminum silicate proppant, which may include the steps of: drying and crushing a raw material containing serpentine minerals to obtain raw material powder; roasting the raw material powder to obtain magnesium aluminum silicate powder; mixing the magnesium aluminum silicate powder with the ingredients to obtain mixed material powder; granulating the mixed material powder to obtain a spherical granular blank; and drying and sintering the spherical granular blank to obtain the magnesium aluminum silicate proppant.
In an exemplary embodiment of the invention, the serpentine mineral-containing feedstock may include one or more of serpentine, serpentine mill tailings, chrysotile mill tailings, and ultrabedrock type metal mineral mill tailings.
In an exemplary embodiment of the present invention, the raw material powder may include, by mass, the raw material powder including, in percentage by mass: 25-40% of MgO and 35-40% of SiO22-10% of CaO, 5-15% of Fe2O31 to 5% of Al2O3The particle diameter of the raw material powder is less than 75 μm.
In an exemplary embodiment of the present invention, the roasting process may be roasting at 650 to 1200 ℃ for 2 to 90min, for example, the roasting may be carried out at a temperature from room temperature to 650 to 1200 ℃ for 2 to 90min at a heating rate of 3 to 20 ℃/min, and the roasting may be carried out in one of roasting kilns including a vertical kiln, a rotary kiln, or a roller kiln.
In an exemplary embodiment of the invention, the ingredient may be an inorganic material powder, and may include one or more of quicklime powder, coal ash powder, coal gangue powder, yellow sand powder, quartz powder, potassium feldspar powder, and illite powder, the addition amount of the ingredient is 15 to 45% of the total mass of the magnesium aluminum silicate powder, and the particle size of the ingredient may be below 75 μm.
In an exemplary embodiment of the present invention, the main crystal phase of the magnesium aluminum silicate powder may be olivine.
In an exemplary embodiment of the present invention, the granulation method may be wet granulation, specifically including: and (2) placing the mixed material powder into a granulator, rotating for 5-20 min at the rotating speed of 0-70 r/min, then adding water and a binder, and continuing to perform rotary granulation for 30-90 min, wherein the adding amount of the water can be 10-15% of the mass of the mixed material powder, and the adding amount of the binder can be 4-20% of the mass of the mixed material powder. And after granulation is finished, shaping for 5-30 min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
In an exemplary embodiment of the present invention, the process of drying the spherical granular green body may include: cooling the tail gas generated by roasting to be lower than 80-120 ℃, and drying the spherical granular blank for 30-90 min by using the cooled tail gas; or drying by a roasting furnace at the drying temperature of 60-90 ℃ for 60-90 min.
In an exemplary embodiment of the present invention, the sintering process may include: raising the temperature from room temperature to 700-850 ℃ at the speed of 5-15 ℃/min, then raising the temperature to 700-1200 ℃ at the speed of 3-7 ℃/min, and keeping the temperature for 3-90 min.
According to another aspect of the invention, the magnesium aluminum silicate proppant can be prepared by adopting the production process as described in any one of the above.
In an exemplary embodiment of the invention, the diameter of the magnesium aluminum silicate proppant is 106-3350 μm, the sphericity and roundness are not lower than 0.9, and the volume density is 0.8-1.65 g/cm3。
The invention further provides application of the magnesium aluminum silicate proppant in oil and gas fracturing.
Compared with the prior art, the beneficial effects of the invention can comprise at least one of the following:
(1) the product takes rocks, waste rocks and tailings mainly containing serpentine as raw materials to produce the high-strength oil fracturing magnesium aluminum silicate proppant, so that the resource utilization of various solid wastes is realized, and the product has important ecological and sustainable development significance on resource protection, saving and high-value utilization;
(2) the recycling of the tailings, the waste rocks and the tailings has important ecological and environmental significance on the safety, environmental protection, reclamation and greenness of the tailings pond;
(3) the production process for obtaining the novel high-strength low-density magnesium aluminum silicate proppant by processing and treating rocks, waste rocks and tailings mainly containing serpentine as raw materials has the advantages of simple production process, energy conservation and emission reduction, high product added value, high ecological environmental benefit and the like, and has important significance for developing new material industry and social economy;
(4) magnesium aluminum silicate powder containing serpentine is roasted to obtain magnesium aluminum silicate powder with olivine as main crystal phase, so that phase transformation of serpentine can be realized, phase inversion detoxification is facilitated, environment is protected, and hardness and strength of the powder can be remarkably improved;
(5) the fracturing propping agent is prepared by using the magnesium aluminum silicate for the first time, so that a good direction is provided for resource utilization of the solid waste containing serpentine;
(6) the strength of the product can be effectively improved, the density of the product is reduced, and the acid corrosion resistance is improved by proportioning, granulating and sintering the mixture;
(7) compared with the traditional proppant, the aluminum magnesium silicate proppant has the advantages that a large amount of quartz sand can be saved, the defects of low strength and poor sphericity of the quartz sand are overcome, the prepared proppant has a wide application pressure range and a wide market prospect;
(8) the prepared magnesium aluminum silicate proppant has the advantages of high strength, low density, high sphericity, good acid corrosion resistance and the like, and has wide market prospect and remarkable economic, environmental and social benefits.
Drawings
Fig. 1 shows a production process flow diagram of an exemplary embodiment 1 of the method according to the invention.
Detailed Description
Hereinafter, the magnesium aluminum silicate proppant of the present invention, its production process and application will be described in detail with reference to the accompanying drawings and exemplary embodiments.
The invention provides a production process for preparing a magnesium aluminum silicate proppant by using a raw material containing serpentine minerals as a raw material through drying, crushing and roasting, a high-strength low-density magnesium aluminum silicate proppant product prepared by the production process, and application of the magnesium aluminum silicate proppant as a proppant in oil and gas exploitation.
Exemplary embodiment 1
As shown in fig. 1, in the present exemplary embodiment, the production process of the magnesium aluminum silicate proppant is realized by the following steps:
and S1, drying and crushing to obtain raw material powder.
Specifically, a raw material containing a serpentine mineral is dried and crushed to obtain a raw material powder. Here, the serpentine mineral-containing raw material may include serpentine-containing rock, waste rock, tailings. Specifically, the raw material may include one or more of serpentine, serpentine tailings, chrysotile tailings, exfoliated serpentine waste, and ultrabasic rock type metal mineral tailings.
The drying process can be carried out in a dryer, and parameters such as the temperature and the time of the dryer are adjusted so that the moisture content of the dried raw material containing the serpentine mineral is less than or equal to 5 percent, such as 2.0 percent and 3.5 percent, and the like, so as to obtain the crushed and dried powder, avoid agglomeration in the crushing process and improve the crushing efficiency. The temperature of the dryer can be 60-120 ℃, and the drying time is 30-150 min. In addition, the drying process can also adopt vacuum drying equipment for drying, so that the drying speed is accelerated, and meanwhile, dust caused by drying can be prevented from diffusing into the air.
The crushing process can be carried out by adopting a closed crushing mode, so that the crushing efficiency is improved, and the uniform granularity can be ensured. The crushing is preferably carried out in a dust-free workshop, so that the environment is protected, and the serpentine fiber can be prevented from diffusing into the environment to cause adverse effects.
The obtained raw material powder mainly contains magnesium silicate powder of serpentine mineral, the water content (free water) of the magnesium silicate powder is below 5%, the water content is controlled in the range, the implementation of subsequent processes can be facilitated, when the water content is higher than 5%, local agglomeration is easy to occur in the roasting process, the roasting uniformity is influenced, the roasting effect is reduced, the crystalline phase conversion of the serpentine powder is not uniform, and the quality of the obtained high-strength low-density proppant product is further influenced.
The obtained raw material powder comprises, by mass, 25-40: 35-40: 2-10: 5-15: 1 to 5 of MgO and SiO2、CaO、Fe2O3And Al2O3. The powder comprises the following chemical components in percentage by mass: 25-40% of MgO and SiO2 35～40％，CaO 2～10％，Fe2O3 5～15％，Al2O3 1～5％，H2O+(bound water) 8-15%.
The particle diameter of the raw material powder is 75 μm or less, for example, 2 to 75 μm. The granularity of the powder body is controlled in the range, so that the certain fineness is ensured, the later granulation is convenient, and the later granulation is influenced by powder agglomeration caused by over-fineness. When the particle size is less than 2 μm, the specific surface area of the raw material powder is too large, the surface energy is high, the powder is easy to agglomerate, and excessive energy is consumed in the production process, which is not economical; when the particle size exceeds 75 μm, although the powder processing cost is reduced, the particle size is too coarse and the specific surface area is too small, so that the roundness, sphericity, compressive strength and uniformity of the product are affected when the magnesium aluminum silicate proppant product is prepared, and in sum, the proper particle size of the raw material powder is preferably less than or equal to 75 μm.
And S2, roasting to obtain the magnesium aluminum silicate powder.
Specifically, the raw material powder obtained in step S1 is calcined to obtain a magnesium aluminum silicate powder having an olivine as a main crystal phase.
The roasting process can be carried out for 2min to 90min when the temperature is raised from the room temperature to 650 ℃ to 1200 ℃, and the temperature raising rate is 3 ℃/min to 20 ℃/min. The roasting can be carried out by adopting one of a vertical kiln, a rotary kiln or a roller kiln. The calcination may also be performed using a calcination kiln commonly used in the art, and will not be described herein in any greater detail. When the calcination temperature is less than 650 ℃, it is difficult to obtain the main olivine crystal phase, and when the temperature is too high, energy is wasted, it is uneconomical, and the calcination time is also so, so that there is an optimum range for both the calcination temperature and the calcination time.
And S3, mixing the powder with the ingredients to obtain mixed material powder.
Specifically, the magnesium aluminum silicate powder obtained in step S2 is mixed with ingredients to obtain a mixed material powder.
The ingredients can be inorganic material powder, and specifically can include one or more of quicklime powder, coal ash powder, coal gangue powder, yellow sand powder, quartz powder, potassium feldspar powder and illite powder, and the addition amount of the ingredients is 15-45% of the total mass of the magnesium aluminum silicate powder. Furthermore, the particle size of the ingredients may be below 75 μm, for example between 2 μm and 75 μm. When the addition amount of the ingredients is less than 15%, the product density is increased, the use quality of the product is influenced, when the addition amount of the ingredients exceeds 45%, the strength of the product is influenced although the density of the obtained product meets the requirement, and when the proportion of the ingredients is within the range of 15-45%, the strength and density requirements of the obtained product can be comprehensively met, so that the product has the best product quality effect. Optionally, the amount of the ingredient added is 30% of the total mass of the magnesium aluminum silicate powder.
And S4, granulating to obtain a spherical granular blank.
Specifically, the mixed material powder obtained in step S3 is granulated to obtain a spherical granular green body.
The granulation process can be wet granulation, the mixed material powder is placed in a granulator and rotates for 5-20 min at the rotating speed of 30-70 r/min, then water and a binder are added, and the granulation is continued for 30-90 min, wherein the adding amount of the water is 10-15% of the mass of the mixed material powder, and the adding amount of the binder is 4-20% of the mass of the mixed material powder. And after granulation is finished, shaping for 5-30 min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
And S5, obtaining the magnesium aluminum silicate proppant.
Specifically, the spherical granular green body obtained in the step S4 is dried and sintered to obtain the high-strength low-density magnesium aluminum silicate proppant. For example, the diameter of the prepared magnesium aluminum silicate proppant is 106-3350 μm, the sphericity and roundness are not less than 0.9, and the volume density is 0.80-1.65 g/cm3The 9% breakage rating is 15K, corresponding to a breakage of not more than 9% at a closure pressure of 103 MPa.
The drying process can be that when the temperature of tail gas generated by roasting in the step S2 is reduced to be lower than 80-120 ℃, the spherical granular blank is dried by utilizing the reduced tail gas, and the drying time is 30-90 min. Drying may also be performed in a kiln to optimize the process and improve efficiency. When the roasting furnace is used for drying, the drying temperature is 60-90 ℃, and the drying time is 60-90 min.
The sintering process can be that the temperature is increased from room temperature to 700-850 ℃ at the speed of 5-15 ℃/min, then the temperature is increased to 700-1200 ℃ at the speed of 3-7 ℃/min, and the temperature is kept for 3-90 min, so as to obtain the magnesium aluminum silicate proppant.
Within the sintering temperature range, a better sintering effect can be achieved, so that the strength of the sintered aluminum-magnesium silicate proppant product is high, the density of the sintered aluminum-magnesium silicate proppant product is low, the strength of the sintered aluminum-magnesium silicate proppant product is difficult to reach the high strength standard when the temperature is lower than 700 ℃, the temperature is higher than 1200 ℃, energy is easily consumed, the density of the sintered aluminum-magnesium silicate proppant product is increased, the product performance and the use quality are reduced, the optimal sintering temperature range exists, the sintering time is also the same, the time is too low, the sintering effect cannot be achieved, the time is too long, the energy is consumed, meanwhile, over-sintering is easily caused, the product density is increased, and the optimal effect cannot be achieved.
The high-strength low-density magnesium aluminum silicate proppant prepared by the invention can reach and exceed various performance standards required by the industry, for example, the crushing rate of the prepared 16-30-mesh magnesium aluminum silicate proppant is 6.8 percent under the 69MPa closed pressure and is lower than the standard of China petrochemical group Petroleum administration enterprisesAccording to the standard requirement of 18% in a fracturing propping agent (QSH 1020-1598-2013), the 9% breakage rate grade can reach 15K according to the proppant performance test method for hydraulic fracturing and gravel packing operation (SY/T5108-2014) in the oil and gas industry standard of the people's republic of China, so that high strength is reflected; the volume density of the prepared 20-40 mesh aluminum-magnesium silicate proppant is 1.60g/cm3Apparent density of 2.26g/cm3And under the closing pressure of 86MPa, the breakage rate is only 5 percent, and the grade of 9 percent breakage rate can reach 15K according to the standard of ' method for testing the performance of proppant for hydraulic fracturing and gravel packing operation ' (SY/T5108-2014) in the oil and gas industry of the people's republic of China.
Exemplary embodiment 2
In the exemplary embodiment, the method for preparing the large-size aragonite whisker by batch carbonization of the calcareous raw material containing impurities can also be realized by the following steps:
1) drying the raw materials containing the serpentine minerals until the water content of each raw material is less than 5%, and crushing to obtain raw material powder, wherein the raw material powder comprises the following components in parts by mass: 35-40: 2-10: 5-15: 1 to 5 of MgO and SiO2、CaO、Fe2O3And Al2O3And the grain diameter of the obtained raw material powder is not less than 2 μm and not more than 75 μm.
2) The raw material powder is roasted in a vertical kiln, a rotary kiln or a pre-decomposition kiln at 650-1200 ℃ for 2-90 min to obtain the magnesium aluminum silicate powder of which the main crystal phase is olivine.
3) And mixing the magnesium aluminum silicate powder with ingredients accounting for 15-45% of the mass sum of the magnesium aluminum silicate powder, wherein the ingredients can comprise one or more of quicklime powder, fly ash powder, coal gangue powder, yellow sand powder, quartz powder, potassium feldspar powder and illite powder to obtain mixed material powder.
4) And (3) rotating the mixed material powder for 5-20 min at the rotating speed of 30-70 r/min in a granulator, then adding water and a binder, and continuing to perform rotary granulation for 30-90 min, wherein the adding amount of the water is 10-15% of the mass of the mixed material powder, and the adding amount of the binder is 4-20% of the mass of the mixed material powder. And after granulation is finished, shaping for 5-30 min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
5) Drying the spherical granular blank in a vertical kiln, a roller kiln or a rotary kiln by tail gas generated by roasting in the step 2), wherein the drying temperature is 60-90 ℃, and the drying time is 60-90 min. And after drying, raising the temperature in the kiln to 900-1200 ℃ at a speed of 10-30 ℃/min, and sintering for 3-90 min to obtain the magnesium aluminum silicate proppant. Drying and sintering may be performed using, but not limited to, a shaft kiln, a roller kiln, or a rotary kiln.
The technical solution of the present invention is further explained by detailed examples below.
Example 1
The specific production process of this example is as follows:
(1) and (3) placing the serpentine beneficiation tailings in a dryer, drying for 50min at 90 ℃, and crushing in a closed-circuit crushing mode to obtain raw material powder with the water content of 3%. The obtained raw material powder comprises 35% of MgO and 40% of SiO27% of CaO, 12% of Fe2O3And 3% of Al2O3The particle size of the raw material powder is 30-75 μm.
(2) And (3) placing the obtained raw material powder in a vertical kiln, heating the raw material powder from room temperature to 950 ℃ at the speed of 10 ℃/min, and roasting the raw material powder for 80min at the temperature to obtain the magnesium aluminum silicate powder of which the main crystal phase is olivine.
(3) Mixing magnesium aluminum silicate powder, quicklime powder and fly ash powder according to the mass ratio of 100: 5: 15, and uniformly mixing in a dry powder mixer for 30min to obtain mixed material powder. Wherein the particle size of the quicklime powder and the fly ash powder is 5-20 μm.
(4) And granulating the mixed material powder by adopting a wet method, wherein the granulating method comprises the steps of rotating the mixed material powder in a granulator for 15min at a rotating speed of 40r/min, then adding water and a binder, and continuously rotating and granulating for 80min, wherein the adding amount of the water is 12% of the mass of the mixed material powder, and the adding amount of the binder is 10% of the mass of the mixed material powder. And after granulation is finished, shaping for 10min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
(5) And (3) drying the spherical granular blank in the vertical kiln for 80min by using the hot tail gas generated by the roasting kiln in the step (2) when the temperature is reduced to 70-80 ℃, then heating to 850 ℃ at a speed of 15 ℃/h, then heating to 1050 ℃ at a speed of 5 ℃/min, and preserving the heat for 40min to obtain a finished product A.
The diameter of the finished product A is between 425 and 850 mu m, the sphericity and roundness are not less than 0.9, and the volume density is 1.1g/cm3The breaking rate is less than or equal to 7% under the closed pressure of 103MPa, the 9% breaking grade is 15K, HCl: HF-12: 3, the acid solubility is less than or equal to 3 percent.
Example 2
The specific production process of this example is as follows:
(1) putting the chrysotile mill tailings into a dryer, drying at 70 ℃ for 120min, and then crushing in a closed-circuit crushing mode to obtain raw material powder with the water content of 4%. The obtained raw material powder comprises 40% of MgO and 35% of SiO26 percent of CaO and 10 percent of Fe2O3And 5% of Al2O3The particle size of the raw material powder is 20-50 μm.
(2) And (3) placing the obtained raw material powder in a roller kiln, heating the raw material powder to 750 ℃ from the room temperature of 20 ℃/min, and roasting the raw material powder for 120min at the temperature to obtain the magnesium aluminum silicate powder of which the main crystalline phase is olivine.
(3) Mixing magnesium aluminum silicate powder, yellow sand powder and potassium feldspar powder according to a mass ratio of 100: 10: 20, and uniformly mixing in a dry powder mixer for 40min to obtain mixed material powder. Wherein the particle size of the yellow sand powder and the potassium feldspar powder is 10-50 mu m.
(4) And (2) granulating the mixed material powder by adopting a wet method, rotating the mixed material powder in a granulator for 10min at the rotating speed of 60r/min, then adding water and a binder, and continuing to perform rotary granulation for 50min, wherein the adding amount of the water is 10% of the mass of the mixed material powder, and the adding amount of the binder is 12% of the mass of the mixed material powder. And after granulation is finished, shaping for 20min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
(5) And (3) drying the spherical granular blank in a vertical kiln for 30min when the temperature is reduced to 110-120 ℃ by utilizing the hot tail gas generated by the roller kiln in the step (2), heating from room temperature to 800 ℃ at the speed of 10 ℃/min, then heating to 1100 ℃ at the speed of 5 ℃/min, and preserving the heat for 25min to obtain a finished product B.
The diameter of the finished product B is between 300 and 600 mu m, the sphericity and roundness are not less than 0.8, and the volume density is 0.9g/cm3The breaking rate is less than or equal to 7% under the closed pressure of 103MPa, the 9% breaking grade is 15K, HCl: HF-12: 3, the acid solubility is less than or equal to 3 percent.
Example 3
The specific production process of this example is as follows:
(1) placing the mineral processing tailings of the super-basic rock type metal mineral products in a dryer at 120 ℃ for drying for 40min, and crushing in a closed-circuit crushing mode to obtain raw material powder with the water content of 2%. The obtained raw material powder comprises 40% of MgO and 40% of SiO28 percent of CaO and 5 percent of Fe2O3And 5% of Al2O3The particle size of the raw material powder is 2-30 μm.
(2) And (3) putting the obtained raw material powder into a rotary kiln, heating the raw material powder to 850 ℃ from room temperature at a speed of 15 ℃/min, and roasting the raw material powder for 100min at the temperature to obtain the magnesium aluminum silicate powder of which the main crystalline phase is olivine.
(3) Mixing magnesium aluminum silicate powder and illite powder according to the mass ratio of 100: 28, and uniformly mixing in a dry powder mixer for 35min to obtain mixed material powder. Wherein the particle size of the illite powder is 30-75 μm.
(4) And (2) granulating the mixed material powder by adopting a wet method, rotating the mixed material powder in a granulator at a rotating speed of 50r/min for 12min, then adding water and a binder, and continuing to perform rotary granulation for 60min, wherein the adding amount of the water is 11% of the mass of the mixed material powder, and the adding amount of the binder is 12% of the mass of the mixed material powder. And after granulation is finished, shaping for 10min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
(5) And (3) drying the spherical granular blank in a rotary kiln for 60min when the temperature is reduced to 90-100 ℃ by utilizing the hot tail gas generated by the roasting kiln in the step (2), heating to 700 ℃ at a speed of 5 ℃/h, heating to 950 ℃ at a speed of 5 ℃/min, and preserving the heat for 100min to obtain a finished product C.
Diameter of finished product CBetween 212 and 425 mu m, the sphericity and roundness are not less than 0.9, and the bulk density is 1.30g/cm3The breaking rate is less than or equal to 5% under the closed pressure of 103MPa, the 9% breaking grade is 15K, HCl: HF-12: 3, the acid solubility is less than or equal to 3 percent.
Example 4
The specific production process of this example is as follows:
(1) drying serpentine in a dryer at 80 ℃ for 100min, and crushing in a closed crushing mode to obtain raw material powder with the water content of 2.5%. The obtained raw material powder comprises 36% of MgO and 38% of SiO29.5 percent of CaO, 11 percent of Fe2O3And 3% of Al2O3The particle size of the raw material powder is 10-50 μm.
(2) And (3) placing the obtained raw material powder in a roller kiln, heating the raw material powder to 1100 ℃ from room temperature at a speed of 10 ℃/min, and roasting the raw material powder for 40min at the temperature to obtain the magnesium aluminum silicate powder of which the main crystalline phase is olivine.
(3) Mixing magnesium aluminum silicate powder and coal gangue powder according to a mass ratio of 100: 25, and uniformly mixing in a dry powder mixer for 20min to obtain mixed material powder. Wherein the particle size of the coal gangue powder is 20-50 μm.
(4) And (2) granulating the mixed material powder by adopting a wet method, rotating the mixed material powder in a granulator for 5min at a rotating speed of 70r/min, then adding water and a binder, and continuing to perform rotary granulation for 35min, wherein the adding amount of the water is 12% of the mass of the mixed material powder, and the adding amount of the binder is 14% of the mass of the mixed material powder. And after granulation is finished, shaping for 10min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
(5) And (3) drying the spherical granular blank in a roller kiln for 40min when the temperature is reduced to 100-110 ℃ by utilizing the hot tail gas generated by the roasting kiln in the step (2), heating to 700 ℃ at a speed of 6 ℃/h, heating to 1000 ℃ at a speed of 6 ℃/min, and preserving the heat for 60min to obtain a finished product D.
The diameter of the finished product D is 425-850 mu m, the sphericity and roundness are not less than 0.9, and the volume density is 1.20g/cm3The breaking rate is less than or equal to 6% under the closed pressure of 103MPa, the 9% breaking grade is 15K, HCl:HF-12: 3, the acid solubility is less than or equal to 3 percent.
Example 5
The specific production process of this example is as follows:
(1) and (3) drying the stripped serpentine waste rock in a dryer at 90 ℃ for 60min, and crushing in a closed-circuit crushing mode to obtain raw material powder with the water content of 2%. The obtained raw material powder comprises 38 percent of MgO and 38 percent of SiO28 percent of CaO, 12 percent of Fe2O3And 2% of Al2O3The particle size of the raw material powder is 20-75 μm.
(2) And (3) placing the obtained raw material powder in a rotary kiln, heating the raw material powder to 1000 ℃ from room temperature at the speed of 7 ℃/min, and roasting the raw material powder for 60min at the temperature to obtain the magnesium aluminum silicate powder of which the main crystalline phase is olivine.
(3) Mixing magnesium aluminum silicate powder and quartz powder according to the mass ratio of 100: 20, and uniformly mixing in a dry powder mixer for 15min to obtain mixed material powder. Wherein the particle size of the quartz powder is 20-75 μm.
(4) And (2) granulating the mixed material powder by adopting a wet method, rotating the mixed material powder in a granulator for 13min at a rotating speed of 50r/min, then adding water and a binder, and continuing to perform rotary granulation for 40min, wherein the adding amount of the water is 13% of the mass of the mixed material powder, and the adding amount of the binder is 8% of the mass of the mixed material powder. And after granulation is finished, shaping for 12min on a spherical shaping machine to obtain a spherical granular blank with better sphericity and roundness.
(5) And (3) drying the spherical granular blank in a rotary kiln for 30min when the temperature is reduced to 110-120 ℃ by utilizing the hot tail gas generated by the roasting kiln in the step (2), heating to 700 ℃ at a speed of 4 ℃/h, heating to 1050 ℃ at a speed of 5 ℃/min, and preserving heat for 50min to obtain a finished product E.
The diameter of the finished product E is between 300 and 600 mu m, the sphericity and roundness are not less than 0.9, and the volume density is 1.30g/cm3The breaking rate is less than or equal to 6% under the closed pressure of 103MPa, the 9% breaking grade is 15K, HCl: HF-12: 3, the acid solubility is less than or equal to 3 percent.
In conclusion, the invention takes rocks, waste rocks and tailings mainly containing serpentine as raw materials to produce the magnesium-aluminum proppant for fracturing petroleum or natural gas, thereby realizing resource utilization of various solid wastes. The magnesium aluminum silicate proppant and the production process thereof have the beneficial effects that at least one of the following components is adopted:
1) rocks, waste rocks and tailings mainly containing serpentine are used as raw materials, and low-grade resources and solid waste residues are utilized; the method has important ecological and sustainable development significance for resource protection, saving and high-value utilization;
2) the production process is simple, energy is saved, emission is reduced, the added value of the product is high, the ecological environment benefit is high, and the like, and the method has important significance for developing new material industry and social economy;
3) the recycling of the tailings, the waste rocks and the tailings has important ecological and environmental significance on the safety, environmental protection, reclamation and greenness of the tailings pond;
4) the volume density of the magnesium aluminum silicate proppant prepared by the production process is 0.80-1.65 g/cm3The grade of 9% breakage rate is 15K, the breakage rate does not exceed 9% under the closing pressure of 103MPa, the applicable pressure range is wide, and the market prospect is wide;
5) the magnesium aluminum silicate proppant prepared by the production process has the advantages of high strength, low density, high sphericity, good acid corrosion resistance and the like, and has wide market prospect and remarkable economic, environmental and social benefits;
6) compared with the traditional proppant, the aluminum magnesium silicate proppant can save a large amount of quartz sand and make up the defects of low strength, poor roundness and poor sphericity of the quartz sand.
Although the present invention has been described above in connection with the exemplary embodiments and the accompanying drawings, it will be apparent to those of ordinary skill in the art that various modifications may be made to the above-described embodiments without departing from the spirit and scope of the claims.
Claims (10)
1. The production process of the magnesium aluminum silicate proppant is characterized by comprising the following steps of:
drying and crushing a raw material containing serpentine minerals to obtain raw material powder;
roasting the raw material powder to obtain magnesium aluminum silicate powder;
mixing the magnesium aluminum silicate powder with the ingredients to obtain mixed material powder;
granulating the mixed material powder to obtain a spherical granular blank;
and drying and sintering the spherical granular blank to obtain the magnesium aluminum silicate proppant.
2. The process for producing a veegum proppant as set forth in claim 1, wherein said serpentine mineral-containing feedstock comprises one or more of serpentine, serpentine mill tailings, chrysotile mill tailings, stripped serpentine rejects, and ultrabasic rock type metal mineral mill tailings.
3. The production process of the magnesium aluminum silicate proppant as set forth in claim 1, wherein the raw material powder comprises, in mass percent: 25-40% of MgO and 35-40% of SiO22-10% of CaO, 5-15% of Fe2O31 to 5% of Al2O3The particle diameter of the raw material powder is less than 75 μm.
4. The production process of the magnesium aluminum silicate proppant as set forth in claim 1, wherein the roasting process is carried out in a roasting kiln comprising a vertical kiln, a rotary kiln or a roller kiln at a temperature rising rate of 3-20 ℃/min from room temperature to 650-1200 ℃ for 2-90 min.
5. The production process of the magnesium aluminum silicate proppant according to claim 1, wherein the ingredients are inorganic material powder, and comprise one or more of quicklime powder, fly ash powder, coal gangue powder, yellow sand powder, quartz powder, potassium feldspar powder and illite powder, the addition amount of the ingredients is 15-45% of the mass sum of the magnesium aluminum silicate powder, and the particle size of the ingredients is less than 75 μm.
6. The process for producing a proppant as set forth in claim 1, wherein the main crystalline phase of the magnesium aluminum silicate powder is olivine.
7. The process for producing the magnesium aluminum silicate proppant as set forth in claim 1, wherein the granulation process is wet granulation, and specifically comprises: placing the mixed material powder in a granulator, and rotating for 5-20 min at the rotating speed of 30-70 r/min; then adding water and a binder, and continuously carrying out rotary granulation for 30-90 min, wherein the adding amount of the water is 10-15% of the mass of the mixed material powder, and the adding amount of the binder is 4-20% of the mass of the mixed material powder; and after granulation is finished, shaping for 5-30 min on a spherical shaping machine to obtain a spherical granular blank.
8. The process for producing a proppant comprising magnesium aluminum silicate as set forth in claim 1, wherein the process for drying the spherical granular green body comprises: cooling the tail gas generated by roasting to be lower than 80-120 ℃, and drying the spherical granular blank for 30-90 min by using the cooled tail gas; or drying by a roasting furnace at the drying temperature of 60-90 ℃ for 60-90 min;
the sintering process comprises the following steps: raising the temperature from room temperature to 700-850 ℃ at the speed of 5-15 ℃/min, then raising the temperature to 700-1200 ℃ at the speed of 3-7 ℃/min, and keeping the temperature for 3-90 min.
9. The magnesium aluminum silicate proppant is characterized by being prepared by the production process of any one of claims 1 to 8, having a diameter of 106 to 3350 μm, a sphericity and a roundness of not less than 0.9, and a bulk density of 0.8 to 1.65g/cm3。
10. Use of the magnesium aluminum silicate proppant of claim 9 in oil and gas fracturing.
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