CN117229039B - Preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength - Google Patents
Preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength Download PDFInfo
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- CN117229039B CN117229039B CN202311498789.3A CN202311498789A CN117229039B CN 117229039 B CN117229039 B CN 117229039B CN 202311498789 A CN202311498789 A CN 202311498789A CN 117229039 B CN117229039 B CN 117229039B
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- 239000010881 fly ash Substances 0.000 title claims abstract description 101
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 43
- -1 rare earth carbonate Chemical class 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 238000000227 grinding Methods 0.000 claims description 25
- 238000007599 discharging Methods 0.000 claims description 21
- NECUCYZCESSQJR-UHFFFAOYSA-H C([O-])([O-])=O.[Ce+3].[La+3].C([O-])([O-])=O.C([O-])([O-])=O Chemical compound C([O-])([O-])=O.[Ce+3].[La+3].C([O-])([O-])=O.C([O-])([O-])=O NECUCYZCESSQJR-UHFFFAOYSA-H 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 238000001694 spray drying Methods 0.000 claims description 13
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000292 calcium oxide Substances 0.000 claims description 12
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 12
- 239000011324 bead Substances 0.000 claims description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 10
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 239000002344 surface layer Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- QCZFMLDHLOYOQJ-UHFFFAOYSA-H samarium(3+);tricarbonate Chemical compound [Sm+3].[Sm+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QCZFMLDHLOYOQJ-UHFFFAOYSA-H 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 3
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims description 3
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 3
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 3
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- AKFFNTKRAYWFRN-UHFFFAOYSA-N ethyl 5-(trifluoromethyl)-1h-pyrazole-3-carboxylate Chemical compound CCOC(=O)C=1C=C(C(F)(F)F)NN=1 AKFFNTKRAYWFRN-UHFFFAOYSA-N 0.000 claims description 2
- RQXZRSYWGRRGCD-UHFFFAOYSA-H gadolinium(3+);tricarbonate Chemical compound [Gd+3].[Gd+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O RQXZRSYWGRRGCD-UHFFFAOYSA-H 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000011810 insulating material Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000011819 refractory material Substances 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract description 2
- 238000010304 firing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 11
- 239000010883 coal ash Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010443 kyanite Substances 0.000 description 1
- 229910052850 kyanite Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000008018 melting Effects 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
- 150000002910 rare earth metals Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Landscapes
- Processing Of Solid Wastes (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength, which comprises the following steps: step 1 is pretreatment of fly ash; step 2, preparing mixed powder; step 3 is the preparation of an anti-adhesion material; step 4 is a firing process. The preparation method of the rare earth carbonate fly ash ceramsite with high barrel pressure strength utilizes the characteristics of rare earth carbonate and the fly ash to prepare the heat-insulating material with light weight, high barrel pressure strength and high refractoriness, expands the application of the rare earth carbonate in the field of heat-insulating and refractory materials of industrial kilns and enriches the downstream industrial chain of the rare earth carbonate; the method can consume a large amount of industrial solid waste fly ash, changes waste into valuable, and solves the problems of environmental pollution and potential safety hazard caused by the storage of the fly ash; the pressure intensity of the fly ash haydite cylinder is improved by more than 40 percent compared with the conventional fly ash haydite cylinder; compared with the conventional fly ash ceramsite material, the heat conductivity coefficient is reduced by more than 30 percent.
Description
Technical Field
The invention belongs to the field of ceramsite, and particularly relates to a preparation method of rare earth carbonate fly ash ceramsite with high cylinder pressure strength.
Background
Fly ash is the main waste of thermal power plants. The method has the advantages of large yield, large occupied area, dust generation, underground water pollution and serious environmental problems.
At present, few ceramsite products can be applied to a high-temperature environment, and less research is performed on improving the cylinder pressure strength of the fly ash ceramsite by utilizing the rare earth carbonate. In order to respond to the ideas of waste-free industry and environment-friendly city, it is necessary to develop a ceramic aggregate product with excellent comprehensive performance by utilizing rare earth carbonate and fly ash.
Disclosure of Invention
In view of the above, the invention aims to overcome the defects in the prior art and provides a preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength comprises the following steps:
step 1 is pretreatment of fly ash: vibrating, roasting at high temperature, grinding and sieving the fly ash to obtain fly ash powder;
step 2 is the preparation of mixed powder: mixing the dried rare earth carbonate with the fly ash powder, performing ball milling and spray drying to obtain mixed powder, and dividing the mixed powder into first powder and second powder;
step 3 is the preparation of an anti-adhesion material: mixing the first powder with a regulator to obtain an anti-adhesion material;
step 4 is a roasting process: and placing the second powder into a granulator, dropwise adding a binder into the second powder, adding an anti-adhesion material into the second powder after the ceramsite is formed, rolling the second powder until the surface layer of the ceramsite is uniformly covered, discharging the second powder, and aging and roasting the second powder to obtain the rare earth carbonate fly ash ceramsite.
Further, the temperature of the drying step in the step 2 is 80-275 ℃ and the time is 1-5h; the rare earth carbonate in the step 2 is at least one of lanthanum carbonate, cerium carbonate, samarium carbonate, gadolinium carbonate, erbium carbonate, yttrium carbonate or lanthanum cerium carbonate; the purity of the rare earth carbonate in the step 2 is more than or equal to 98 percent.
Further, the linear speed of the ball milling step in the step 2 is 1-13m/s, the temperature is 15-40 ℃, the solid content is 25-80%, and the grain diameter of ground slurry is 1 mu m less than or equal to D 90 Less than or equal to 3 mu m; the feeding speed of the spray drying step in the step 2 is 0.1-60L/min, the temperature is 210-280 ℃, and the particle size of the powder after spray drying is 7 mu m less than or equal to D 90 ≤13μm。
Further, the mass ratio of the dried rare earth carbonate to the fly ash powder in the step 2 is 1-15:85-99.
Further, the mass of the regulator in the step 3 is 0.1-20w% of the first powder; the regulator in the step 3 is at least one of alumina, silica, calcium oxide or graphite powder; the mixing step in the step 3 is carried out for 0.1-2h.
Further, the binder in the step 4 is at least one of water, water glass, aluminum dihydrogen phosphate or high-temperature sol; the high-temperature sol is at least one of silica sol, aluminum sol or zirconium sol; the mass ratio of the binder to the second powder in the step 4 is 15-28:72-85.
Further, the inclination angle of the granulator in the step 4 is 30-50 degrees, and the rotating speed is 10-60rpm; the speed of the dripping step in the step 4 is 0.0001-10L/s; the diameter of the ceramsite in the step 4 is 3-30mm; the addition amount of the anti-adhesion material in the step 4 is 1-10w% of the ceramsite.
Further, the temperature of the aging step in the step 4 is 18-30 ℃, the humidity is 35-65%, and the time is 8-24 hours; the parameters of the roasting step in the step 4 are as follows: heating from room temperature to 200deg.C at a rate of 5-30deg.C/min, maintaining at 200deg.C for 15-300min, heating from 200deg.C to 1100-1450 deg.C at a rate of 3-10deg.C/min, maintaining for 1-150min, and cooling to room temperature.
Further, the classification of the shaking step in the step 1 is 17-28K, and floating beads with the size of more than 300 mu m are sieved; the temperature of the high-temperature roasting step in the step 1 is 750-900 ℃ and the time is 1-5h; the particle size of the grinding step in the step 1 is 1200 meshes, and the residual rate is less than or equal to 5%.
Further, the fly ash in the step 1 consists of the following components in percentage by mass: 10-45% of aluminum oxide, 25-55% of silicon oxide, less than or equal to 15% of calcium oxide, less than or equal to 5% of magnesium oxide, less than or equal to 7% of ferric oxide and less than or equal to 5% of potassium sodium.
The rare earth carbonate is decomposed into rare earth oxide at about 900 ℃, and CO is continuously generated in the process 2 At the temperature, the coal ash material starts to generate a low-melting-point liquid phase, but the coal ash material cannot form effective packages on the gas due to the low content, so that part of the gas escapes along a rare earth carbonate decomposition gas path in the stage of burning expansion at 1100 ℃, and the closed pores formed by the final ceramsite are small and dense, and have larger barrel pressure strength compared with the common burning expansion ceramsite.
The rare earth carbonate promotes the decomposition of the sodium feldspar and the potassium feldspar with low melting points in the fly ash at high temperature, and the rare earth oxide generated by the high-temperature decomposition of the rare earth carbonate in the reaction process can promote the generation of a low-melting-point liquid phase, can provide a more sufficient ion thermal motion environment for an aluminum phase and a silicon phase, and promotes the aluminum-silicon phase to generate a kyanite phase and a cristobalite phase at a lower temperature, so that the strength of the ceramsite skeleton component is further enhanced, and the pressure performance of a ceramsite cylinder is enhanced.
Compared with the prior art, the invention has the following advantages:
the preparation method of the rare earth carbonate fly ash ceramsite with high barrel pressure strength utilizes the characteristics of rare earth carbonate and the fly ash to prepare the heat-insulating material with light weight, high barrel pressure strength and high refractoriness, expands the application of the rare earth carbonate in the field of heat-insulating and refractory materials of industrial kilns and enriches the downstream industrial chain of the rare earth carbonate; the method can consume a large amount of industrial solid waste fly ash, changes waste into valuable, and solves the problems of environmental pollution and potential safety hazard caused by the storage of the fly ash; the pressure intensity of the fly ash haydite cylinder is improved by more than 40 percent compared with the conventional fly ash haydite cylinder; compared with the conventional fly ash ceramsite material, the heat conductivity coefficient is reduced by more than 30 percent.
Drawings
FIG. 1 is a graph of rare earth carbonate fly ash ceramsite and fly ash ceramsite according to example 1 of the present invention.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
A preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength comprises the following steps:
(1) The fly ash is taken and classified by 17K vibration, floating beads above 300 microns are removed, the rest of the screened fly ash is discharged and air-cooled to 25 ℃ after being roasted for 5 hours at 800 ℃, the fly ash is taken and ground by a high-energy air flow mill, the 1200 mesh sieve is taken for discharging, and the components of the fly ash after grinding are 26 percent of alumina, 45 percent of silica, 11 percent of calcium oxide, 3 percent of magnesium oxide, 6.05 percent of ferric oxide and 1.25 percent of potassium sodium;
(2) Mixing lanthanum cerium carbonate 80g and coal ash 1940g which are dried at 270 ℃ for 2 hours into 50 percent of solid content, feeding the mixture into a ball mill for high-energy grinding, wherein the linear speed is 8m/s, the discharging temperature is 25 ℃, and grinding until D is reached 90 Spray drying at feed rate of 2L/min at thermal spray temperature of 270 ℃, D after drying 90 Mixed micropowder with particle diameter of 10 μm;
(3) 60g of mixed micro powder is taken and added with 6g of alpha-alumina, and the mixture is fully mixed for 30min in a three-dimensional powder mixer to obtain an anti-sticking layer material;
(4) And (3) filling the rest mixed micro powder into a granulator, setting the rotating speed to be 20rpm, uniformly dripping 500g of neutral water, uniformly adding an anti-adhesion material when the diameter d=15 mm of the ceramsite is about, rolling until the surface layer of the ceramsite is uniformly covered with the anti-adhesion material, discharging, and aging for 14 hours at the temperature of 25 ℃ and the humidity of 45%. And (3) placing the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1255 ℃ at 5 ℃/min, and preserving heat for 180min to obtain the cerium lanthanum carbonate fly ash sintered and expanded ceramsite, wherein the spectrogram of the cerium lanthanum carbonate fly ash sintered and expanded ceramsite is shown in figure 1.
Example 2
A preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength comprises the following steps:
(1) The fly ash is taken and classified by 17K vibration, floating beads above 300 microns are removed, the rest of the screened fly ash is discharged and air-cooled to 25 ℃ after being roasted for 5 hours at 800 ℃, the fly ash is taken and ground by a high-energy air flow mill, the 1200 mesh sieve is taken for discharging, and the components of the fly ash after grinding are 26 percent of alumina, 45 percent of silica, 11 percent of calcium oxide, 3 percent of magnesium oxide, 6.05 percent of ferric oxide and 1.25 percent of potassium sodium;
(2) Taking lanthanum carbonate 76g, samarium carbonate 70g and coal ash 1940g which are dried at 270 ℃ for 2 hours and mixed into 50 percent of solid content, feeding the mixture into a ball mill for high-energy grinding, wherein the linear speed is 8m/s, the discharging temperature is 25 ℃, and grinding until D is reached 90 Spray drying at feed rate of 2L/min at thermal spray temperature of 270 ℃, D after drying 90 Mixed micropowder with particle diameter of 10 μm;
(3) Adding 60g of mixed micropowder into 4g of alpha-alumina and 2g of silicon oxide, and fully mixing in a three-dimensional powder mixer for 30min to obtain an anti-bonding layer material;
(4) And (3) filling the rest mixed micro powder into a granulator, setting the disc surface to incline by 35 degrees, setting the rotating speed to be 20rpm, uniformly dripping 500g of aluminum sol (5%), uniformly adding 66g of anti-bonding material when the diameter d=15 mm of the ceramsite is about, rolling until the surface layer of the ceramsite is uniformly covered and discharged, and aging for 14 hours at the temperature of 25 ℃ and the humidity of 45%. And (3) placing the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1285 ℃ at 5 ℃/min, and preserving heat for 130min to obtain the cerium lanthanum carbonate fly ash sintered and expanded ceramsite.
Example 3
A preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength comprises the following steps:
(1) The fly ash is taken and classified by 17K vibration, floating beads above 300 microns are removed, the rest of the screened fly ash is discharged and air-cooled to 25 ℃ after being roasted for 5 hours at 800 ℃, the fly ash is taken and ground by a high-energy air flow mill, the 1200 mesh sieve is taken for discharging, and the components of the fly ash after grinding are 26 percent of alumina, 45 percent of silica, 11 percent of calcium oxide, 3 percent of magnesium oxide, 6.05 percent of ferric oxide and 1.25 percent of potassium sodium;
(2) Taking 192g of samarium carbonate which is dried at 270 ℃ for 2 hours, 100 g of cerium carbonate and 1800g of fly ash which are mixed to form 50 percent of solid content, feeding the mixture into a ball mill for high-energy grinding, wherein the linear speed is 8m/s, the discharging temperature is 25 ℃, and grinding until D is reached 90 Spray drying at feed rate of 2L/min at thermal spray temperature of 270 ℃, D after drying 90 Mixed micropowder with particle diameter of 10 μm;
(3) Adding 60g of mixed micropowder into 5g of alpha-alumina and 2g of silicon oxide, and fully mixing in a three-dimensional powder mixer for 30min to obtain an anti-bonding layer material;
(4) And (3) filling the rest mixed micro powder into a granulator, setting the disc surface to incline by 35 degrees, setting the rotating speed to be 20rpm, uniformly dripping 450g of aluminum dihydrogen phosphate (10%), uniformly adding 67g of anti-bonding material when the diameter d=15 mm of the ceramsite is about, rolling until the surface layer of the ceramsite is uniformly covered and discharged, and aging for 14 hours at the temperature of 25 ℃ and the humidity of 45%. And (3) placing the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1285 ℃ at 5 ℃/min, and preserving heat for 120min to obtain the cerium lanthanum carbonate fly ash sintered and expanded ceramsite.
Comparative example 1
A preparation method of fly ash ceramsite comprises the following steps:
(1) The fly ash is taken and classified by 17K vibration, floating beads above 300 microns are removed, the rest of the screened fly ash is discharged and air-cooled to 25 ℃ after being roasted for 5 hours at 800 ℃, the fly ash is taken and ground by a high-energy air flow mill, the 1200 mesh sieve is taken for discharging, and the components of the fly ash after grinding are 26 percent of alumina, 45 percent of silica, 11 percent of calcium oxide, 3 percent of magnesium oxide, 6.05 percent of ferric oxide and 1.25 percent of potassium sodium;
(2) 2020g of fly ash is proportioned into 50% solid content, and then the mixture is put into a ball mill for high-energy grinding, the linear speed is 8m/s, the discharging temperature is 25 ℃, and the mixture is ground to D 90 Spray drying treatment was performed at =3μm, andthe material speed is 2L/min, the thermal spraying temperature is 270 ℃, and D is obtained after drying 90 Micropowder with particle diameter of 10 μm;
(3) Putting the rest of the micro powder into a granulator, tilting the disc surface by 35 degrees, setting the rotating speed to 20rpm, uniformly dripping 500g of neutral water, uniformly adding 66g of the anti-adhesion material prepared in the example 1 when the diameter d=15 mm of the ceramsite is about, rolling until the surface layer of the ceramsite is uniformly covered with the anti-adhesion material, discharging, and aging for 14 hours at the temperature of 25 ℃ and the humidity of 45%. And (3) placing the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1255 ℃ at 5 ℃/min, and preserving heat for 180min to obtain the fly ash sintered and expanded ceramsite, wherein the spectrogram of the fly ash sintered and expanded ceramsite is shown in figure 1.
Comparative example 2
A preparation method of rare earth carbonate fly ash ceramsite comprises the following steps:
(1) Taking fly ash, roasting the fly ash for 5 hours at the high temperature of 800 ℃, discharging, air-cooling to 25 ℃, grinding the fly ash by a high-energy air flow mill, and taking the fly ash with 1200 meshes for discharging, wherein the components of the fly ash after grinding are 26% of alumina, 45% of silica, 11% of calcium oxide, 3% of magnesia, 6.05% of ferric oxide and 1.25% of potassium sodium;
(2) Mixing lanthanum cerium carbonate 80g and coal ash 1940g which are dried at 270 ℃ for 2 hours into 50 percent of solid content, feeding the mixture into a ball mill for high-energy grinding, wherein the linear speed is 8m/s, the discharging temperature is 25 ℃, and grinding until D is reached 90 Spray drying at feed rate of 2L/min at thermal spray temperature of 270 ℃, D after drying 90 Mixed micropowder with particle diameter of 10 μm;
(3) Putting the rest mixed micro powder into a granulator, tilting the disc surface by 35 degrees, setting the rotating speed to 20rpm, uniformly dripping 500g of neutral water, uniformly adding 66g of the anti-adhesion material prepared in the example 1 when the diameter d=15 mm of the ceramsite is about, rolling until the surface layer of the ceramsite is uniformly covered with the anti-adhesion material, discharging, and aging for 14 hours at the temperature of 25 ℃ and the humidity of 45%. After aging, the ceramsite is filled into a muffle furnace, the temperature is increased to 200 ℃ at 10 ℃/min, the temperature is kept for 30min at 200 ℃, the temperature is increased to 1255 ℃ at 5 ℃/min, and the temperature is kept for 180min, so that the ceramsite cannot be obtained, because the raw material of the non-impurity-removed fly ash contains low-melting glass beads and a large amount of fluxing alkali metal, and the ceramsite cannot be kept in a spherical shape after being roasted at 1255 ℃ and melted and liquefied.
Comparative example 3
A preparation method of rare earth carbonate fly ash ceramsite comprises the following steps:
(1) The fly ash is taken and classified by 17K vibration, floating beads above 300 microns are removed, the rest of the screened fly ash is subjected to high-temperature roasting at 800 ℃ for 5 hours, then the discharged fly ash is subjected to air cooling to 25 ℃ for discharging, and the components of the ground fly ash are 26% of alumina, 45% of silica, 11% of calcium oxide, 3% of magnesia, 6.05% of ferric oxide and 1.25% of potassium sodium;
(2) Mixing 80g of lanthanum cerium carbonate dried at 270 ℃ for 2h with 1940g of fly ash, loading into a granulator, tilting the disc surface by 35 ℃, setting the rotating speed to 20rpm, uniformly dripping 500g of neutral water, uniformly adding 66g of the anti-adhesion material prepared in the example 1 when the diameter d=15 mm of the ceramsite is about, rolling until the surface layer of the ceramsite is uniformly covered and discharged, and ageing at the temperature of 25 ℃ and the humidity of 45% for 14h. After aging, the ceramsite is put into a muffle furnace, the temperature is increased to 200 ℃ at 10 ℃/min, the temperature is kept for 30min at 200 ℃, the temperature is increased to 1255 ℃ at 5 ℃/min, and the temperature is kept for 180min, so that the cerium lanthanum carbonate fly ash sintered and expanded ceramsite can be obtained, the microstructure of the cerium lanthanum carbonate fly ash mixed powder material is not uniform enough, the sintered and expanded pores are unevenly distributed, pores are easily distributed on the surface layer of the ceramsite, and the core layer of the ceramsite is free from pores.
Comparative example 4
A preparation method of rare earth carbonate fly ash ceramsite comprises the following steps:
(1) The fly ash is taken and classified by 17K vibration, floating beads above 300 microns are removed, the rest of the screened fly ash is discharged and air-cooled to 25 ℃ after being roasted for 5 hours at 800 ℃, the fly ash is taken and ground by a high-energy air flow mill, the 1200 mesh sieve is taken for discharging, and the components of the fly ash after grinding are 26 percent of alumina, 45 percent of silica, 11 percent of calcium oxide, 3 percent of magnesium oxide, 6.05 percent of ferric oxide and 1.25 percent of potassium sodium;
(2) Mixing lanthanum cerium carbonate 80g and coal ash 1940g which are dried at 270 ℃ for 2 hours into 50 percent of solid content, feeding the mixture into a ball mill for high-energy grinding, wherein the linear speed is 8m/s, the discharging temperature is 25 ℃, and grinding until D is reached 90 Spray drying at feed rate of 2L/min at thermal spray temperature of 270 ℃, D after drying 90 Mixed micropowder with particle diameter of 10 μm;
(3) The mixed micro powder is put into a granulator, the disc surface is inclined by 35 degrees, the rotating speed is set to 20rpm, the neutral water is evenly dripped into 500g, the mixture is discharged when the diameter d of the ceramsite is about 15mm, and the mixture is aged for 14 hours at the temperature of 25 ℃ and the humidity of 45 percent. And (3) placing the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1255 ℃ at 5 ℃/min, and preserving heat for 180min to obtain the cerium lanthanum carbonate fly ash sintered and expanded ceramsite.
Comparative example 5
A preparation method of rare earth carbonate fly ash ceramsite comprises the following steps:
(1) The fly ash is taken and classified by 17K vibration, floating beads above 300 microns are removed, the rest of the screened fly ash is discharged and air-cooled to 25 ℃ after being roasted for 5 hours at 800 ℃, the fly ash is taken and ground by a high-energy air flow mill, the 1200 mesh sieve is taken for discharging, and the components of the fly ash after grinding are 26 percent of alumina, 45 percent of silica, 11 percent of calcium oxide, 3 percent of magnesium oxide, 6.05 percent of ferric oxide and 1.25 percent of potassium sodium;
(2) Mixing lanthanum cerium carbonate 80g and coal ash 1940g which are dried at 270 ℃ for 2 hours into 50 percent of solid content, feeding the mixture into a ball mill for high-energy grinding, wherein the linear speed is 8m/s, the discharging temperature is 25 ℃, and grinding until D is reached 90 Spray drying at feed rate of 2L/min at thermal spray temperature of 270 ℃, D after drying 90 Mixed micropowder with particle diameter of 10 μm;
(3) And (3) filling the rest mixed micro powder into a granulator, setting the rotating speed to be 20rpm, uniformly dripping 500g of neutral water, uniformly adding 66g of alpha-alumina when the diameter d=15 mm of the ceramsite is about, rolling until the surface layer of the ceramsite is uniformly covered and discharged, and aging for 14h at the temperature of 25 ℃ and the humidity of 45%. After aging, the ceramsite is put into a muffle furnace, the temperature is increased to 200 ℃ at 10 ℃/min, the temperature is kept for 30min at 200 ℃, the temperature is increased to 1255 ℃ at 5 ℃/min, the temperature is kept for 180min, and the cerium lanthanum carbonate fly ash sintered and expanded ceramsite can be obtained, and the thermal expansibility and the refractoriness matching property of the alumina regulator are greatly different from those of a ceramsite matrix, so that the ceramsite is not expanded completely and cannot be sintered.
The performance test was performed on each example and each comparative example, and the results are shown in table 1.
Table 1 performance data table
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (5)
1. A preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength is characterized by comprising the following steps: the method comprises the following steps:
step 1 is pretreatment of fly ash: vibrating, roasting at high temperature, grinding and sieving the fly ash to obtain fly ash powder;
step 2 is the preparation of mixed powder: mixing the dried rare earth carbonate with the fly ash powder, performing ball milling and spray drying to obtain mixed powder, and dividing the mixed powder into first powder and second powder;
step 3 is the preparation of an anti-adhesion material: mixing the first powder with a regulator to obtain an anti-adhesion material;
step 4 is a roasting process: placing the second powder into a granulator, dropwise adding a binder into the second powder, adding an anti-adhesion material into the second powder after the ceramsite is formed, rolling the second powder until the surface layer of the ceramsite is uniformly covered, discharging the second powder, and aging and roasting the second powder to obtain the rare earth carbonate fly ash ceramsite;
the temperature of the drying step in the step 2 is 80-275 ℃ and the time is 1-5h; the rare earth carbonate in the step 2 is at least one of lanthanum carbonate, cerium carbonate, samarium carbonate, gadolinium carbonate, erbium carbonate, yttrium carbonate or lanthanum cerium carbonate; the purity of the rare earth carbonate in the step 2 is more than or equal to 98 percent;
the mass ratio of the dried rare earth carbonate to the fly ash powder in the step 2 is 1-15:85-99;
the mass of the regulator in the step 3 is 0.1-20w% of the first powder; the regulator in the step 3 is at least one of alumina, silica or calcium oxide; the time of the mixing step in the step 3 is 0.1-2h;
the inclination angle of the granulator in the step 4 is 30-50 degrees, and the rotating speed is 10-60rpm; the speed of the dripping step in the step 4 is 0.0001-10L/s; the diameter of the ceramsite in the step 4 is 3-30mm; the addition amount of the anti-adhesion material in the step 4 is 1-10% by weight of the ceramsite;
the classification of the vibration step in the step 1 is 17-28K, and floating beads with the particle size of more than 300 μm are sieved; the temperature of the high-temperature roasting step in the step 1 is 750-900 ℃ and the time is 1-5h; the particle size of the grinding step in the step 1 is 1200 meshes, and the residual rate is less than or equal to 5%.
2. The method for preparing the high-cylinder-pressure-strength rare earth carbonate fly ash ceramsite, which is characterized by comprising the following steps of: the linear speed of the ball milling step in the step 2 is 1-13m/s, the temperature is 15-40 ℃, the solid content is 25-80%, and the particle size of ground slurry is 1 mu m less than or equal to D 90 Less than or equal to 3 mu m; the feeding speed of the spray drying step in the step 2 is 0.1-60L/min, the temperature is 210-280 ℃, and the particle size of the powder after spray drying is 7 mu m less than or equal to D 90 ≤13μm。
3. The method for preparing the high-cylinder-pressure-strength rare earth carbonate fly ash ceramsite, which is characterized by comprising the following steps of: the binder in the step 4 is at least one of water, water glass, aluminum dihydrogen phosphate or high-temperature sol; the high-temperature sol is at least one of silica sol, aluminum sol or zirconium sol; the mass ratio of the binder to the second powder in the step 4 is 15-28:72-85.
4. The method for preparing the high-cylinder-pressure-strength rare earth carbonate fly ash ceramsite, which is characterized by comprising the following steps of: the temperature of the aging step in the step 4 is 18-30 ℃, the humidity is 35-65%, and the time is 8-24h; the parameters of the roasting step in the step 4 are as follows: heating from room temperature to 200deg.C at a rate of 5-30deg.C/min, maintaining at 200deg.C for 15-300min, heating from 200deg.C to 1100-1450 deg.C at a rate of 3-10deg.C/min, maintaining for 1-150min, and cooling to room temperature.
5. The method for preparing the high-cylinder-pressure-strength rare earth carbonate fly ash ceramsite, which is characterized by comprising the following steps of: the fly ash in the step 1 consists of the following components in percentage by mass: 10-45% of aluminum oxide, 25-55% of silicon oxide, less than or equal to 15% of calcium oxide, less than or equal to 5% of magnesium oxide, less than or equal to 7% of ferric oxide and less than or equal to 5% of potassium sodium.
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