CN117466635B - 一种稀土改性煤矸石制备致密莫来石的方法 - Google Patents
一种稀土改性煤矸石制备致密莫来石的方法 Download PDFInfo
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- CN117466635B CN117466635B CN202311824071.9A CN202311824071A CN117466635B CN 117466635 B CN117466635 B CN 117466635B CN 202311824071 A CN202311824071 A CN 202311824071A CN 117466635 B CN117466635 B CN 117466635B
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- mullite
- ball milling
- rare earth
- gangue
- oxide
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- 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 title claims abstract description 68
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 25
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 68
- 238000005245 sintering Methods 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 20
- -1 rare earth compound Chemical class 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 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 20
- 239000003245 coal Substances 0.000 claims description 19
- 239000004568 cement Substances 0.000 claims description 14
- 230000004913 activation Effects 0.000 claims description 13
- 229910001570 bauxite Inorganic materials 0.000 claims description 12
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims description 12
- 150000004706 metal oxides Chemical class 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 9
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- 229910003440 dysprosium oxide Inorganic materials 0.000 claims description 4
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 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
- 230000003213 activating effect Effects 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 239000000378 calcium silicate Substances 0.000 claims description 2
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 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
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 2
- WMOHXRDWCVHXGS-UHFFFAOYSA-N [La].[Ce] Chemical compound [La].[Ce] WMOHXRDWCVHXGS-UHFFFAOYSA-N 0.000 abstract description 9
- LENJPRSQISBMDN-UHFFFAOYSA-N [Y].[Ce] Chemical compound [Y].[Ce] LENJPRSQISBMDN-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000843 powder Substances 0.000 description 33
- 239000000203 mixture Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 13
- 238000000465 moulding Methods 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- 239000010935 stainless steel Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000002910 solid waste Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000005065 mining Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- JTUZZGLMVUXHQL-UHFFFAOYSA-N [Y].[Sm] Chemical compound [Y].[Sm] JTUZZGLMVUXHQL-UHFFFAOYSA-N 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000005641 tunneling Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
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Abstract
本发明提供了一种稀土改性煤矸石制备致密莫来石的方法,包括如下步骤:将活化煤矸石、稀土复合物、铝源、球磨溶剂经球磨混料、烘干、破碎、成型、高温烧结后制得致密莫来石。本发明所制备的莫来石成本低廉,相较电熔莫来石成本降低50%左右,相较于添加氧化稀土的烧结莫来石,添加锆酸镧铈和铝酸铈钇的烧结莫来石致密度更高,孔隙率最低可至0.96%,体积密度最高可达到3.05g/cm³,莫来石含量超过90%。
Description
技术领域
本发明属于莫来石制备领域,尤其是涉及一种稀土改性煤矸石制备致密莫来石的方法。
背景技术
莫来石是由铝硅酸盐组成的,在高温下生成的矿物统称,莫来石矿被用来生产高温耐火原材料。天然的莫来石矿物很稀少,天然的莫来石晶体为细长的针状且呈放射簇状。莫来石是Al2O3-SiO2 ,密度:≥2.65g/cm3,莫氏硬度:6~7 耐火度: 1790°C时仍很稳定。通常使用的莫来石都是人工合成的,合成莫来石是一种很好的耐火材料,其具有膨胀均匀、热震稳定性好、荷重软化点高、高温蠕变值小、硬度大、耐化学腐蚀性好等等优点。
目前所使用的莫来石通常用烧结法或者电熔法人工合成。合成莫来石的种类主要有天普通烧结莫来石、普通电熔莫来石、高纯电熔莫来石。
烧结法的工艺为烧结莫来石通常采用较好的天然铝矾土为原料,经精选工序,经1750℃以上高温回转窖烧结而成。烧结法按照原材料制备的方式又分为干法工艺与湿法工艺。干法工艺是将配料共同粉磨,经压球或压坯后用回转窑或隧道窑烧成;湿法工艺是将配合料加水磨成浆,再压滤脱水成为泥饼,真空挤泥成为泥段或泥坯再经烧成。合成莫来石对所用原材料的纯度要求很严格,少量杂质成分就会降低莫来石的含量。影响烧结法合成莫来石的主要工艺因素是原材料的纯度、细度和煅烧温度。
电熔法的工艺为电熔法是将配料放在电弧炉里,在电弧炉形成的高温中熔融,冷却析晶而成,采用原料配料时可不经过粉磨直接将块状原料破碎至小于2.0mm的颗粒,(比如铝矾土等材料)再与其他粉状原料在混合机里混合均匀。电熔莫来石与烧结莫来石相比较而言,电熔莫来石晶体发育完善,晶粒大、缺陷少,同时高温力学性能和耐侵蚀性要好。
而想要制备高纯致密莫来石通常使用氧化铝、二氧化硅、高铝矾土等成本较高的矿物为原料,按照一定比例,进行极高温度下烧结,从而制备出较为高纯致密的莫来石材料。而此种方法成本较高,极大限制了致密莫来石的市场应用。
煤矸石是矿业固体废物的一种,是在掘进、开采和洗煤过程中排出的固体废物。是矿业固体废物的一种,包括洗煤厂的洗矸、煤炭生产中的手选矸、半煤巷和岩巷掘进中排出的煤和岩石以及和煤矸石一起堆放的煤系之外的白矸等的混合物。是碳质、泥质和砂质页岩的混合物,具有低发热值。含碳20%~30%,有些含腐殖酸。煤矸石中的硫化物逸出或浸出会污染大气、农田和水体。矸石山还会自燃发生火灾,或在雨季崩塌,淤塞河流造成灾害。故如何利用煤矸石是近年来的研究热点。
发明内容
有鉴于此,本发明旨在克服现有技术中的缺陷,提出一种稀土改性煤矸石制备致密莫来石的方法。
为达到上述目的,本发明的技术方案是这样实现的:
一种稀土改性煤矸石制备致密莫来石的方法,包括如下步骤:将活化煤矸石、稀土复合物、铝源、球磨溶剂经球磨混料、烘干、破碎、成型、高温烧结后制得致密莫来石,其中,所述稀土复合物的制备方法如下:将第一金属氧化物和第二金属氧化物混合后,在高温下进行固相合成得到稀土复合物,反应温度为500℃-1200℃,反应时间为1-4h,升温速率为1-10℃/min,所述第一金属氧化物为氧化铝和/或氧化锆,所述第二金属氧化物为氧化铈、氧化镧、氧化钇、氧化钐、氧化钕、氧化镝中两种或两种以上。
优选地,所述第一金属氧化物和第二金属氧化物的质量比为(1~5):(1~5)。
优选地,所述的活化煤矸石、稀土复合物、铝源质量比为(1~3):(0.1~0.5):(0.5~2)。
优选地,所述活化煤矸石的制备方法如下:将煤矸石原料经过高能活化或者高温活化得到活化煤矸石,所述高能活化的转速为300-800rad/min,时间为4-8h,所述高温活化的温度为600℃-800℃,时间为2-4h。
优选地,所述的铝源为氧化铝、氢氧化铝、高铝矾土中的一种或几种。铝源的作用是补充煤矸石中的铝元素,保证莫来石的完全合成。
优选地,所述的球磨溶剂为水或乙醇。
优选地,所述球磨混料为湿法球磨或干法球磨中的一种;球磨转速为150rad/min-450rad/min,球磨时间为1h-24h。
优选地,所述烘干温度为80℃-120℃,烘干时间为2 h-24 h。
优选地,所述高温烧结的烧结温度为1250℃-1650℃,烧结时间为1 h-6 h,升温速率为1℃/min-10℃/min。
优选地,所述高温烧结过程中添加粘结剂,所述粘结剂为水、铝酸钙水泥、硅酸钙水泥、硅溶胶、PVA、PVB、PVP中的一种或几种。
本发明采用固体废弃物煤矸石为主要原料,同时,煤矸石由于为固体废弃物,故而其成本极低。首先对原料煤矸石进行活化,通过活化使煤矸石形成更多的不定型二氧化硅和不定型氧化铝,从而可以更好的促进莫来石的合成反应。稀土复合物为将氧化铝、氧化锆中的一种和氧化铈、氧化镧、氧化钇、氧化钐、氧化钕、氧化镝中的两种,在高温下进行固相合成为稀土复合化合物,采用稀土复合化合物的优点为通过不同的稀土与硅、铝、氧可以更好更快的形成低熔点固溶体,低熔点固溶体在高温下呈液态,而金属离子在液态中可以更为有效和快速的进行扩散,而且不同的稀土形成的低熔点固溶体的熔点有所差异,因此可以通过相同温度下更好的控制铝离子、硅离子、氧离子的扩散速率,即避免了反应过快导致莫来石过烧,气孔率较高,也避免了低温下莫来石反应不完全的情况,从而更好的控制莫来石反应速率,使得反应更为完全、可控,同时使莫来石可以在更低的温度下形成。而铝离子、锆离子进入莫来石晶格内,替换原来的硅离子、铝离子,从而是晶格更为稳定,使致密度更高,同时锆离子和铝离子也会同氧离子、硅离子等形成复合氧化物,进一步提高了莫来石的形成致密度。进而在较低的温度下即可制备出低成本、环保、低碳的高纯致密莫来石。
相对于现有技术,本发明具有以下优势:
本发明所制备的莫来石成本低廉,相较电熔莫来石成本降低50%左右,相较于添加氧化稀土的烧结莫来石,添加锆酸镧铈和铝酸铈钇的烧结莫来石致密度更高,孔隙率最低可至0.96%,体积密度最高可达到3.05g/cm³,莫来石含量超过90%。
附图说明
图1为实施例4制得的成品的微观电镜图;
图2为对比例1制得的成品的微观电镜图。
具体实施方式
除有定义外,以下实施例中所用的技术术语具有与本发明创造所属领域技术人员普遍理解的相同含义。以下实施例中所用的试验试剂,如无特殊说明,均为常规生化试剂;所述实验方法,如无特殊说明,均为常规方法。
下面结合实施例来详细说明本发明。
实施例1
称取煤矸石粉在800℃进行高温活化2h后,取出降温,将氧化铝、氧化镧、氧化铈按照4:5:5的质量比混合均匀后在1000℃下烧结3h得到铝酸镧铈,然后将105g活化煤矸石、12g铝酸镧铈、133g氢氧化铝粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间1小时,球磨转速300rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:30:8的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1300℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为3.58%,体积密度为2.87g/cm³,莫来石含量约为90%。
实施例2
称取煤矸石粉放入球磨罐,在800rad/min下进行高能活化12h后,取出烘干,将氧化锆、氧化钇、氧化铈按照6:7:7的质量比混合均匀后在1200℃下烧结2h得到锆酸铈钇,将136g活化煤矸石、17g锆酸铈钇、97g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间1.5小时,球磨转速300rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:20:8的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1400℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为2.43%,体积密度为2.91g/cm³,莫来石含量约为94%。
实施例3
称取煤矸石粉在700℃进行高温活化3h后,取出降温,将氧化铝、氧化钐、氧化钇按照6:5:5的质量比混合均匀后在1000℃下烧结4h得到铝酸钐钇,将180g活化煤矸石、10g铝酸钐钇、50g氧化铝粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为1.99%,体积密度为2.96g/cm³,莫来石含量约为95%。
实施例4
称取煤矸石粉在700℃进行高温活化3h后,取出降温,将氧化锆、氧化铈、氧化镧按照2:5:5的质量比混合均匀后在1000℃下烧结4h得到锆酸镧铈,将125g活化煤矸石、15g锆酸镧铈、110g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为1.38%,体积密度为3.01g/cm³,莫来石含量约为93%。
实施例5
称取煤矸石粉在700℃进行高温活化3h后,取出降温,将氧化铝、氧化铈、氧化钇按照10:1:1的质量比混合均匀后在1000℃下烧结4h得到铝酸铈钇,将200g活化煤矸石、30g铝酸铈钇、150g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为3.52%,体积密度为2.89g/cm³,莫来石含量约为94%。
实施例6
称取煤矸石粉在700℃进行高温活化3h后,取出降温,将氧化铝、氧化钕、氧化镝按照10:3:3的质量比混合均匀后在1000℃下烧结4h得到铝酸钕镝,将300g活化煤矸石、50g铝酸钕镝、200g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为0.96%,体积密度为3.05g/cm³,莫来石含量约为90%。
对比例1:
称取煤矸石粉在700℃进行高温活化3h后,取出降温,将125g活化煤矸石、15g氧化镧、110g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为5.37%,体积密度为2.50g/cm³,莫来石含量约为86%。
对比例2:
称取煤矸石粉在700℃进行高温活化3h后,取出降温,将氧化锆、氧化镧按照2:5的质量比混合均匀后在1000℃下烧结4h得到锆酸镧,将125g活化煤矸石、15g锆酸镧、110g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为5.34%,体积密度为2.63g/cm³,莫来石含量约为84%。
对比例3:
将氧化锆、氧化铈、氧化镧按照2:5:5的质量比混合均匀后在1000℃下烧结4h得到铝酸铈钇,将125g煤矸石、15g锆酸镧铈、110g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为4.72%,体积密度为2.71g/cm³,莫来石含量约为85%。
对比例4:
称取125g煤矸石粉在700℃进行高温活化3h后,取出降温,将125g活化煤矸石、6g氧化锆、5g氧化铈、5g氧化镧、110g高铝矾土粉放入球磨罐,向球磨罐内注入500ml水,进行湿法球磨,球磨时间2小时,球磨转速250rad/min,将球磨混料倒出在110℃烘干后,破碎成粉,将混料粉体、水、铝酸钙水泥按质量比例:100:25:6的比例混合均匀后,倒入条状不锈钢模具内成型,带样条干燥后放入马弗炉内在1350℃下,升温速率为5℃/min,高温烧结3小时,结束后带样条冷却后取出。该样条经测试孔隙率为4.02%,体积密度为2.81g/cm³,莫来石含量约为86%。
实施例4制得的成品的微观电镜图如图1所示,对比例1制得的成品的微观电镜图如图2所示,可以看出,添加了锆酸镧铈的莫来石中柱状莫来石颗粒明显多于添加氧化镧的莫来石,且氧化铝颗粒和不定型硅铝酸盐明显更少,说明了添加锆酸镧铈更加有助于莫来石的反应形成。
以上所述仅为本发明创造的较佳实施例而已,并不用以限制本发明创造,凡在本发明创造的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明创造的保护范围之内。
Claims (6)
1.一种稀土改性煤矸石制备致密莫来石的方法,其特征在于:包括如下步骤:将活化煤矸石、稀土复合物、铝源、球磨溶剂经球磨混料、烘干、破碎、成型、高温烧结后制得致密莫来石,其中,所述稀土复合物的制备方法如下:将第一金属氧化物和第二金属氧化物混合后,在高温下进行固相合成得到稀土复合物,反应温度为1000℃-1200℃,反应时间为1-4h,升温速率为1-10℃/min,所述第一金属氧化物为氧化铝和/或氧化锆,所述第二金属氧化物为氧化铈、氧化镧、氧化钇、氧化钐、氧化钕、氧化镝中两种或两种以上;
所述第一金属氧化物和第二金属氧化物的质量比为1:5;
所述的活化煤矸石、稀土复合物、铝源质量比为(1~3):(0.1~0.5):(0.5~2);
所述活化煤矸石的制备方法如下:将煤矸石原料经过高能活化或者高温活化得到活化煤矸石,所述高能活化的转速为300-800rad/min,时间为4-8h,所述高温活化的温度为600℃-800℃,时间为2-4h;
所述高温烧结的烧结温度为1250℃-1650℃,烧结时间为1 h-6 h,升温速率为1℃/min-10℃/min。
2.根据权利要求1所述的稀土改性煤矸石制备致密莫来石的方法,其特征在于:所述的铝源为氧化铝、氢氧化铝、高铝矾土中的一种或几种。
3.根据权利要求1所述的稀土改性煤矸石制备致密莫来石的方法,其特征在于:所述的球磨溶剂为水或乙醇。
4.根据权利要求1所述的稀土改性煤矸石制备致密莫来石的方法,其特征在于:所述球磨混料为湿法球磨,球磨转速为150rad/min-450rad/min,球磨时间为1h-24h。
5.根据权利要求1所述的稀土改性煤矸石制备致密莫来石的方法,其特征在于:所述烘干温度为80℃-120℃,烘干时间为2 h-24 h。
6.根据权利要求1所述的稀土改性煤矸石制备致密莫来石的方法,其特征在于:所述高温烧结过程中添加粘结剂,所述粘结剂为水、铝酸钙水泥、硅酸钙水泥、硅溶胶、PVA、PVB、PVP中的一种或几种。
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