CN117229041B - Method for preparing light ceramsite by using rare earth halide solution modifier - Google Patents
Method for preparing light ceramsite by using rare earth halide solution modifier Download PDFInfo
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- CN117229041B CN117229041B CN202311499178.0A CN202311499178A CN117229041B CN 117229041 B CN117229041 B CN 117229041B CN 202311499178 A CN202311499178 A CN 202311499178A CN 117229041 B CN117229041 B CN 117229041B
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- rare earth
- oxide
- halide solution
- ceramsite
- fly ash
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- -1 rare earth halide Chemical class 0.000 title claims abstract description 63
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 56
- 239000003607 modifier Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000010881 fly ash Substances 0.000 claims abstract description 54
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 239000011324 bead Substances 0.000 claims description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000292 calcium oxide Substances 0.000 claims description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 8
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 8
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 5
- ONLCZUHLGCEKRZ-UHFFFAOYSA-N cerium(3+) lanthanum(3+) oxygen(2-) Chemical compound [O--].[O--].[O--].[La+3].[Ce+3] ONLCZUHLGCEKRZ-UHFFFAOYSA-N 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 4
- 229940075630 samarium oxide Drugs 0.000 claims description 4
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 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 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 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 2
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 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
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 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 2
- 238000007873 sieving Methods 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 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
- 238000005245 sintering Methods 0.000 abstract description 2
- CNERRGRDMYRHEV-UHFFFAOYSA-H [Cl-].[La+3].[Ce+3].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] Chemical compound [Cl-].[La+3].[Ce+3].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] CNERRGRDMYRHEV-UHFFFAOYSA-H 0.000 description 8
- 239000012071 phase Substances 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- FHPXUAVVGMAZKL-UHFFFAOYSA-N lanthanum(3+) oxygen(2-) samarium(3+) Chemical compound [O-2].[Sm+3].[La+3].[O-2].[O-2] FHPXUAVVGMAZKL-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012360 testing method 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
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for preparing light ceramsite by utilizing a rare earth halide solution modifier, which comprises the following steps: step 1 is pretreatment of fly ash; step 2, preparing a rare earth halide solution modifier; step 3 is a balling process. The method for preparing the light ceramsite by using the rare earth halide solution modifier provided by the invention has the advantages that the sintering temperature of the light ceramsite is reduced by more than 16% compared with that of the traditional fly ash ceramsite, and the energy is saved.
Description
Technical Field
The invention belongs to the field of ceramsite, and particularly relates to a method for preparing light ceramsite by using a rare earth halide solution modifier.
Background
The rare earth halide is a general name of a compound formed by combining rare earth elements and halogen elements, such as rare earth fluoride, rare earth chloride, rare earth bromide and the like, has low melting point, hygroscopicity and easy dissolution in water, and is not reported in the literature at present for preparing light ceramsite.
The Chinese patent (201810196846.5) with publication No. CN108383540A discloses a method for loading rare earth oxide into pore canal on the surface of fly ash ceramic by alkaline cleaning, dipping and roasting to realize Cr treatment in sewage 6+ Is removed.
The invention of Chinese patent with publication number CN115504803A (202211119278.1) discloses a fly ash-based cordierite honeycomb ceramic and a preparation method thereof, wherein the honeycomb ceramic is prepared by adding binder, plasticizer, dispersant and water into fly ash and other inorganic batching powder. Rare earth fluoride auxiliary agent is added, so that the ceramic has excellent thermal and mechanical properties.
At present, few ceramsite products can be applied to a high-temperature environment, and the porosity research of preparing the lightweight fly ash ceramsite by utilizing the rare earth halide solution is less. Therefore, in response to the ideas of waste-free industry and environment-friendly city, it is quite necessary to develop a light ceramsite product with excellent comprehensive performance by utilizing the rare earth halide solution modifier and the fly ash.
Disclosure of Invention
In view of the above, the present invention aims to overcome the defects in the prior art, and provides a method for preparing light ceramsite by using a rare earth halide solution modifier.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a method for preparing light ceramsite by utilizing rare earth halide solution modifier comprises the following steps:
step 1 is pretreatment of fly ash: vibrating, roasting, grinding and sieving the fly ash to obtain fly ash powder;
step 2 is to prepare rare earth halide solution modifier: adding a rare earth compound into the heated acid liquor, regulating the pH value of the solution, filtering after the reaction is completed, heating the obtained filtrate, continuously stirring the filtrate after crystallization, filtering the crystal after the reaction is completed, adding deionized water into the crystal, and uniformly mixing to obtain the rare earth halide solution modifier;
step 3 is a balling process: placing fly ash powder into a granulator, dropwise adding the rare earth halide solution modifier into the fly ash powder, and then aging and roasting the prepared ceramsite to obtain the light ceramsite.
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 roasting step in the step 1 is 750-900 ℃ and the time is 1-5h; the screen residue rate of the grinding step in the step 1 after the grinding step passes through a 1200-mesh screen is less than or equal to 5 percent. Calcination is used to remove carbon residue.
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.
Further, the rare earth compound in the step 2 is rare earth oxide or rare earth carbonate; the rare earth oxide is at least one of lanthanum oxide, cerium oxide, samarium oxide, yttrium oxide, lanthanum cerium oxide or samarium oxide; the rare earth carbonate is at least one of lanthanum carbonate, cerium carbonate, samarium carbonate, yttrium carbonate, cerium lanthanum carbonate or samarium lanthanum carbonate; the purity of the rare earth compound in the step 2 is more than or equal to 4N.
Further, the pH value in the step 2 is 6-7; the acid liquor in the step 2 is hydrochloric acid or hydrobromic acid; the concentration of the hydrochloric acid is 18-19wt%; the concentration of the hydrobromoacid is 16.5-18wt%; the temperature of the acid liquor in the step 2 is 65-85 ℃; the temperature of the heating step in the step 2 is 125-150 ℃; the stirring step in the step 2 has a speed of 1-60rpm.
Further, the mass ratio of the rare earth compound to the acid liquor in the step 2 is 1-2:1-2; the concentration of the rare earth halide solution modifier in the step 2 is 80-400g/L.
Further, the solid-to-liquid ratio of the fly ash powder in the step 1 to the rare earth halide solution modifier in the step 3 is (72-85) g: (15-28) mL.
Further, the inclination angle of the granulator in the step 3 is 30-50 degrees, and the rotating speed is 10-60rpm; the speed of the dripping step in the step 3 is 0.0001-10L/s; the diameter of the ceramsite in the step 3 is 1.5-15mm.
Further, the temperature of the aging step in the step 3 is 18-30 ℃, the humidity is 35-65%, and the time is 8-24h.
Further, the parameters of the roasting step in the step 3 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 900-1350 deg.C at a rate of 3-10deg.C/min, maintaining for 1-150min, and cooling to room temperature.
The rare earth in the rare earth halide solution exists in an ionic state, and is more fully mixed than a solid material in the process of uniformly dripping the rare earth into the ball, so that the air holes are more uniformly distributed in the process of firing and expanding the ceramsite. The rare earth halide has a relatively low melting point, and a low melting point liquid phase is generated at a relatively low temperature to provide a more sufficient ion thermal motion environment for an aluminum phase and a silicon phase, so that the aluminum phase and the silicon phase are promoted to generate a mullite phase at the relatively low temperature, and meanwhile, the low melting point liquid phase has a certain viscosity and can be preferentially coated on the surface of ceramsite, so that gas generated by gas forming components in the ceramsite is locked in a plastic deformation mode, and each sealed pore is formed. The rare earth halide ceramsite can be further deliquesced in the aging process to generate hydroxide, part of hydroxide in the solution can react with aluminum ions, the existence of aluminum hydroxide can increase the reaction between aluminum and a silicon-rich phase, and a more sufficient mullite phase generation environment is provided, so that the introduction of the rare earth halide can improve the closed porosity of the fly ash ceramsite.
Compared with the prior art, the invention has the following advantages:
the method for preparing the light ceramsite by using the rare earth halide solution modifier provided by the invention has the advantages that the sintering temperature of the light ceramsite is reduced by more than 16% compared with that of the traditional fly ash ceramsite, and the energy is saved.
Compared with the traditional fly ash ceramsite, the lightweight ceramsite has the advantages that the stacking density is reduced by more than 60%.
The lightweight ceramsite disclosed by the invention has higher porosity and the number of pores is increased by 40%.
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 method for preparing light ceramsite by utilizing rare earth halide solution modifier comprises the following steps:
(1) The fly ash is subjected to 17K vibration classification, floating beads above 300 microns are removed, the rest of the screened fly ash is subjected to 800 ℃ roasting for 5 hours, then is discharged and air-cooled to 25 ℃, is subjected to high-energy air flow grinding, and 1940g of fly ash powder is taken out of a 1200 mesh sieve after grinding, wherein the components of the powder comprise 29% of alumina, 43% of silica, 9% of calcium oxide, 3% of magnesia, 6.27% of ferric oxide and 1.55% of potassium sodium;
(2) Placing 5L of hydrochloric acid in a high-temperature reaction kettle, stirring and heating to 70 ℃, adding 3000g of lanthanum cerium oxide in batches, adjusting the pH value of the solution to be 6 until the solution is completely clarified, taking out the solution, filtering insoluble impurities, adding the filtrate into the high-temperature reaction kettle, stirring and heating again to 150 ℃, adjusting the stirring rotation speed to 20rpm after the solution is crystallized, closing the heating, cooling to 25 ℃, crystallizing, carrying out suction filtration on the solution, filtering out all crystals, and adding purified water to adjust the concentration to 120g/L to obtain the lanthanum cerium chloride solution;
(3) Putting the fly ash powder into a granulator, setting the disc surface to incline by 35 degrees, setting the rotating speed to 20rpm, uniformly dripping 120 g/L500 ml of lanthanum cerium chloride solution, discharging until the diameter d=15 mm of the ceramsite is about, ageing at 25 ℃ and 45% of humidity for 14 hours, putting the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1050 ℃ at 5 ℃/min, preserving heat for 22min, and cooling to room temperature to obtain the lanthanum cerium chloride solution modified fly ash light ceramsite.
Example 2
A method for preparing light ceramsite by utilizing rare earth halide solution modifier comprises the following steps:
(1) The fly ash is subjected to 17K vibration classification, floating beads above 300 microns are removed, the rest of the screened fly ash is subjected to 800 ℃ roasting for 5 hours, then discharged and air-cooled to 25 ℃, and is subjected to high-energy air flow grinding, and 1900g of fly ash powder is taken out of 1200 mesh sieve after grinding, wherein the components of the powder comprise 29% of alumina, 43% of silica, 9% of calcium oxide, 3% of magnesia, 6.27% of ferric oxide and 1.55% of potassium sodium;
(2) Placing 5L of hydrochloric acid in a high-temperature reaction kettle, stirring and heating to 70 ℃, adding 3000g of samarium lanthanum oxide in batches, adjusting the pH value of the solution to be 6 until the solution is completely clarified, taking out the solution, filtering insoluble impurities, adding the filtrate into the high-temperature reaction kettle, stirring and heating again to 150 ℃, adjusting the stirring rotation speed to 20rpm after crystallization of the solution occurs, closing heating, cooling to 25 ℃, crystallizing, carrying out suction filtration on the solution, filtering out all crystals, and adding purified water to adjust the concentration to 200g/L to obtain the samarium lanthanum chloride solution;
(3) Putting the fly ash powder into a granulator, setting the disc surface to incline by 35 degrees, setting the rotating speed to 20rpm, uniformly dripping 200 g/L500 ml of samarium lanthanum chloride solution, discharging when the diameter d=15 mm of the ceramsite is about, ageing at 25 ℃ and 45% of humidity for 14 hours, putting the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1035 ℃ at 5 ℃/min, preserving heat for 20min, and cooling to room temperature to obtain the samarium lanthanum chloride solution modified fly ash light ceramsite.
Example 3
A method for preparing light ceramsite by utilizing rare earth halide solution modifier comprises the following steps:
(1) The fly ash is subjected to 17K vibration classification, floating beads above 300 microns are removed, the rest of the screened fly ash is subjected to 800 ℃ roasting for 5 hours, then discharged and air-cooled to 25 ℃, and is subjected to high-energy air flow grinding, and after grinding, 1860g of fly ash powder is taken from 1200 mesh screen blanking, wherein the components comprise 29% of alumina, 43% of silica, 9% of calcium oxide, 3% of magnesia, 6.27% of ferric oxide and 1.55% of potassium sodium;
(2) Placing 5L of hydrochloric acid in a high-temperature reaction kettle, stirring and heating to 70 ℃, adding 3000g of samarium lanthanum carbonate in batches, adjusting the pH value of the solution to be 6 until the solution is completely clarified, taking out the solution, filtering insoluble impurities, adding the filtrate into the high-temperature reaction kettle, stirring and heating again to 150 ℃, adjusting the stirring rotation speed to 20rpm after the solution is crystallized, closing the heating, cooling to 25 ℃, crystallizing, carrying out suction filtration on the solution, filtering out all crystals, and adding purified water to adjust the concentration to 280g/L to obtain the samarium lanthanum chloride solution;
(3) Loading the fly ash powder into a granulator, tilting the disc surface by 35 degrees, setting the rotating speed to 20rpm, uniformly dripping 280 g/L500 ml of samarium lanthanum chloride solution, discharging until the diameter d=15 mm of the ceramsite is about, ageing at 25 ℃ and 45% of humidity for 14 hours, loading the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1030 ℃ at 5 ℃/min, preserving heat for 20min, and cooling to room temperature to obtain the samarium lanthanum chloride solution modified fly ash light ceramsite.
Comparative example 1
A method for preparing light ceramsite, comprising the following steps:
(1) The fly ash is subjected to 17K vibration classification, floating beads above 300 microns are removed, the rest of the screened fly ash is subjected to 800 ℃ roasting for 5 hours, then discharged and air-cooled to 25 ℃, and 2000g of fly ash powder is taken as the powder of the 1200 mesh screen after grinding, wherein the components of the powder comprise 29% of alumina, 43% of silica, 9% of calcium oxide, 3% of magnesia, 6.27% of ferric oxide and 1.55% of potassium sodium;
(2) Putting the fly ash powder into a granulator, setting the rotating speed to be 20rpm, uniformly dripping 500ml of neutral water, discharging until the diameter d=15 mm of the ceramsite is about, ageing at 25 ℃ and 45% of humidity for 14 hours, putting the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1030 ℃ at 5 ℃/min, preserving heat for 20min, and cooling to room temperature to obtain the fly ash ceramsite.
Comparative example 2 (sodium chloride was added instead of lanthanum cerium chloride)
A method for preparing light ceramsite, comprising the following steps:
(1) The fly ash is subjected to 17K vibration classification, floating beads above 300 microns are removed, the rest of the screened fly ash is subjected to 800 ℃ roasting for 5 hours, then is discharged and air-cooled to 25 ℃, is subjected to high-energy air flow grinding, and 1940g of fly ash powder is taken out of a 1200 mesh sieve after grinding, wherein the components of the powder comprise 29% of alumina, 43% of silica, 9% of calcium oxide, 3% of magnesia, 6.27% of ferric oxide and 1.55% of potassium sodium;
(2) Putting the fly ash powder into a granulator, tilting the disc surface by 35 degrees, setting the rotating speed to 20rpm, uniformly dripping 120 g/L500 ml of sodium chloride solution, discharging until the diameter d=15 mm of the ceramsite is about, ageing at 25 ℃ and 45% of humidity for 14 hours, putting the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1030 ℃ at 5 ℃/min, preserving heat for 20min, cooling to room temperature, and melting the ceramsite, wherein the ceramsite cannot be formed. (sodium chloride melting point 801 ℃, excessive liquid phase causes the proportion of framework components in the high-temperature state of the ceramsite to be reduced, fusion liquefaction occurs, and the sphericity cannot be maintained).
Comparative example 3 (powder particle size control was not performed)
A method for preparing light ceramsite by utilizing rare earth halide solution modifier comprises the following steps:
(1) The fly ash is subjected to 17K vibration classification, floating beads above 300 microns are removed, the rest of the screened fly ash is roasted for 5 hours at 800 ℃, and then discharged, 1940g of fly ash powder is taken, and the components of the powder comprise 29% of alumina, 43% of silica, 9% of calcium oxide, 3% of magnesia, 6.27% of ferric oxide and 1.55% of potassium sodium;
(2) Placing 5L of hydrochloric acid in a high-temperature reaction kettle, stirring and heating to 70 ℃, adding 3000g of lanthanum cerium oxide in batches, adjusting the pH value of the solution to be 6 until the solution is completely clarified, taking out the solution, filtering insoluble impurities, adding the filtrate into the high-temperature reaction kettle, stirring and heating again to 150 ℃, adjusting the stirring rotation speed to 20rpm after the solution is crystallized, closing the heating, cooling to 25 ℃, crystallizing, carrying out suction filtration on the solution, filtering out all crystals, and adding purified water to adjust the concentration to 120g/L to obtain the lanthanum cerium chloride solution;
(3) Putting the fly ash powder into a granulator, setting the disc surface to incline by 35 degrees, setting the rotating speed to 20rpm, uniformly dripping 120 g/L500 ml of lanthanum cerium chloride solution, discharging until the diameter d=15 mm of the ceramsite is about, ageing at 25 ℃ and 45% of humidity for 14 hours, putting the aged ceramsite into a muffle furnace, heating to 200 ℃ at 10 ℃/min, preserving heat for 30min at 200 ℃, heating to 1050 ℃ at 5 ℃/min, preserving heat for 22min, and cooling to room temperature to obtain the lanthanum cerium chloride solution modified fly ash ceramsite. (lanthanum chloride cerium fly ash mixed powder material has uneven microstructure, uneven distribution of burning and expanding pores and easy pore distribution on the surface layer of the ceramsite, and no pore generation of the core layer of the ceramsite)
The ceramsite products obtained in each example and each comparative example were tested, 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 (7)
1. A method for preparing light ceramsite by using rare earth halide solution modifier is characterized in that: the method comprises the following steps:
step 1 is pretreatment of fly ash: vibrating, roasting, grinding and sieving the fly ash to obtain fly ash powder;
step 2 is to prepare rare earth halide solution modifier: adding a rare earth compound into the heated acid liquor, regulating the pH value of the solution, filtering after the reaction is completed, heating the obtained filtrate, continuously stirring the filtrate after crystallization, filtering the crystal after the reaction is completed, adding deionized water into the crystal, and uniformly mixing to obtain the rare earth halide solution modifier;
step 3 is a balling process: placing fly ash powder into a granulator, dropwise adding the rare earth halide solution modifier into the fly ash powder, and aging and roasting the prepared ceramsite to obtain the light ceramsite;
the rare earth compound in the step 2 is rare earth oxide or rare earth carbonate; the rare earth oxide is at least one of lanthanum oxide, cerium oxide, samarium oxide, yttrium oxide, lanthanum cerium oxide or samarium oxide; the rare earth carbonate is at least one of lanthanum carbonate, cerium carbonate, samarium carbonate, yttrium carbonate, cerium lanthanum carbonate or samarium lanthanum carbonate;
the parameters of the roasting step in the step 3 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 900-1350 deg.C at a rate of 3-10deg.C/min, maintaining for 1-150min, and cooling to room temperature;
the screen residue rate of the grinding step in the step 1 after passing through a 1200-mesh screen is less than or equal to 5%;
the acid liquor in the step 2 is hydrochloric acid or hydrobromic acid;
the mass ratio of the rare earth compound to the acid liquor in the step 2 is 1-2:1-2; the concentration of the rare earth halide solution modifier in the step 2 is 80-400g/L;
the solid-liquid ratio of the fly ash powder in the step 1 to the rare earth halide solution modifier in the step 3 is 72-85:15-28.
2. The method for preparing light ceramsite by using rare earth halide solution modifier as set forth in claim 1, wherein: the classification of the shaking step in the step 1 is 17-28K, and floating beads with the diameter of more than 300 mu m are removed; the roasting step in the step 1 is carried out at 750-900 ℃ for 1-5h.
3. The method for preparing light ceramsite by using rare earth halide solution modifier as set forth in claim 1, wherein: 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.
4. The method for preparing light ceramsite by using rare earth halide solution modifier as set forth in claim 1, wherein: the purity of the rare earth compound in the step 2 is more than or equal to 4N.
5. The method for preparing light ceramsite by using rare earth halide solution modifier as set forth in claim 1, wherein: the pH value in the step 2 is 6-7; the concentration of the hydrochloric acid is 18-19wt%; the concentration of the hydrobromoacid is 16.5-18wt%; the temperature of the acid liquor in the step 2 is 65-85 ℃; the temperature of the heating step in the step 2 is 125-150 ℃; the stirring step in the step 2 has a speed of 1-60rpm.
6. The method for preparing light ceramsite by using rare earth halide solution modifier as set forth in claim 1, wherein: the inclination angle of the granulator in the step 3 is 30-50 degrees, and the rotating speed is 10-60rpm; the speed of the dripping step in the step 3 is 0.0001-10L/s; the diameter of the ceramsite in the step 3 is 1.5-15mm.
7. The method for preparing light ceramsite by using rare earth halide solution modifier as set forth in claim 1, wherein: the temperature of the aging step in the step 3 is 18-30 ℃, the humidity is 35-65%, and the time is 8-24h.
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