CN117466622A - 一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法 - Google Patents
一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法 Download PDFInfo
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- CN117466622A CN117466622A CN202311503247.0A CN202311503247A CN117466622A CN 117466622 A CN117466622 A CN 117466622A CN 202311503247 A CN202311503247 A CN 202311503247A CN 117466622 A CN117466622 A CN 117466622A
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- Prior art keywords
- fly ash
- rare earth
- earth oxide
- ceramsite
- oxide
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- 239000010881 fly ash Substances 0.000 title claims abstract description 83
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011812 mixed powder Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001694 spray drying Methods 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 3
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 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 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- 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 13
- 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
- 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
- 238000007667 floating Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 6
- 229940075630 samarium oxide Drugs 0.000 claims description 6
- 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 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 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
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 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
- 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
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000007599 discharging Methods 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- -1 Rare earth fluoride Chemical class 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000011148 porous material Substances 0.000 description 3
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000010883 coal ash Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QLBLBSQSYJYIFV-UHFFFAOYSA-N [O-2].[La+3].[O-2].[Y+3] Chemical compound [O-2].[La+3].[O-2].[Y+3] QLBLBSQSYJYIFV-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 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
- 239000002956 ash Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 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
- 229910052906 cristobalite Inorganic materials 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
- 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 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 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
- 238000010304 firing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 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
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 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
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
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- C04B33/135—Combustion residues, e.g. fly ash, incineration waste
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Abstract
本发明提供了一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,包括如下步骤:步骤1是粉煤灰的前处理:将粉煤灰进行震荡、高温焙烧、研磨、过筛后得到;步骤2是陶粒的制备:将稀土氧化物进行球磨、喷雾干燥后与所述的粉煤灰粉体进行共混后得到混合粉体;步骤3是成球工艺:将所述的混合粉体置于造粒机中,将粘结剂均匀滴加入所述的混合粉体中,然后将制得的陶粒进行陈化、焙烧后得到所述的稀土氧化物粉煤灰陶粒。本发明所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法添加稀土氧化物制备的粉煤灰陶粒具备更高的荷重软化温度,较未添加稀土氧化物的陶粒荷重软化温度提高10%以上。
Description
技术领域
本发明属于陶粒领域,尤其是涉及一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法。
背景技术
粉煤灰是火力发电厂的主要废弃物,我国煤的平均粉煤灰产出量是26-30kg/t。每一万千瓦发电排灰渣量约0.9-1.0万吨。其产量大、占地多,并且成扬尘,污染地下水,造成非常严重的环境问题。稀土氧化物应用领域非常广泛,可作为抛光粉、催化剂、储氢材料、玻璃陶瓷、PVC助剂、稀土合金等。
公开号为CN108383540A的中国发明授权专利(申请号为201810196846.5),公开了一种通过碱洗浸渍、高温焙烧方式将稀土氧化物负载在粉煤灰陶瓷表面孔道中,实现对污水中Cr6+的去除。公开号为CN115504803A的中国专利发明申请(申请号为202211119278.1),公开了粉煤灰基堇青石蜂窝陶瓷及其制备方法,由粉煤灰与其他无机配料粉体外加粘结剂、塑性剂、分散剂和水制成。加入了稀土氟化物助剂,使得陶瓷热学及力学性能优异。
目前,可应用于高温环境下陶粒产品很少,利用稀土氧化物提高粉煤灰陶粒气孔率研究更少。因此,响应无废工业、环保城市理念,利用稀土氧化物粉煤灰陶粒开发一种综合性能优良的陶粒产品相当有必要。
发明内容
有鉴于此,本发明旨在克服现有技术中的缺陷,提出一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法。
为达到上述目的,本发明的技术方案是这样实现的:
一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,包括如下步骤:
步骤1是粉煤灰的前处理:将粉煤灰进行震荡、高温焙烧、研磨、过筛后得到;
步骤2是陶粒的制备:将稀土氧化物进行球磨、喷雾干燥后与所述的粉煤灰粉体进行共混后得到混合粉体;
步骤3是成球工艺:将所述的混合粉体置于造粒机中,将粘结剂均匀滴加入所述的混合粉体中,然后将制得的陶粒进行陈化、焙烧后得到所述的稀土氧化物粉煤灰陶粒。
进一步,所述的步骤2中的稀土氧化物为氧化镧、氧化铈、氧化钐、氧化钇、氧化镧铈或氧化镧钐中的至少一种;所述的步骤2中的稀土氧化物的纯度REO≥98%;所述的步骤2中的稀土氧化物的固含量为25-80%。
进一步,所述的步骤2中的球磨步骤的线速度为1-13m/s,温度为15-40℃,研磨后的料浆的粒径为500nm≤D90≤1000nm;所述的步骤2中的喷雾干燥步骤的进料速度为0.1-60L/min,温度为210-280℃,喷雾干燥后的粉体的粒径为1μm≤D90≤5μm。
进一步,所述的步骤2中经喷雾干燥后的稀土氧化物粉体与所述的粉煤灰粉体的质量比为1-12:88-99。
进一步,所述的步骤3中的粘结剂为水、水玻璃、磷酸二氢铝、硅溶胶、铝溶胶或锆溶胶中的至少一种;所述的步骤3中的粘结剂与所述的混合粉体的质量比为15-28:72-85。
进一步,所述的步骤3中的造粒机的倾斜角为30°-50°,转速为10-60rpm;所述的步骤3的滴加步骤的速率为0.0001-10L/s;所述的步骤3中的陶粒的直径为1.5-15mm。
进一步,所述的步骤3中的陈化步骤的温度为18-30℃,湿度为35-65%,时间为8-24h。
进一步,所述的步骤3中的焙烧步骤的参数如下:以5-30℃/min的速率由室温升温至200℃,200℃保温15-300min,以3-10℃/min的速率由200℃升温至1100-1350℃,保温1-150min后冷却至室温。
进一步,所述的步骤1中的震荡步骤的分级为17-28K,筛分出300μm以上的漂珠;所述的步骤1中的高温焙烧步骤的温度为750-900℃,时间为1-5h;所述的步骤1中的研磨步骤过1200目筛网后的筛余率≤5%。
进一步,所述的步骤1中的粉煤灰由包括如下质量百分比的组分组成:氧化铝10-45%,氧化硅25-55%,氧化钙≤15%,氧化镁≤5%,氧化铁≤7%,钾钠≤5%。
相对于现有技术,本发明具有以下优势:
本发明所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法添加稀土氧化物制备的粉煤灰陶粒具备更高的荷重软化温度,较未添加稀土氧化物的陶粒荷重软化温度提高10%以上;稀土氧化物与粉煤灰中硅铝组分在高温时生成硅酸稀土、铝酸稀土,反应过程中的低熔点液相会给铝相、硅相提供更充分的离子热运动环境,促使铝硅相在较低温度下生成蓝晶石相、方石英相、莫来石相从而具备更高的荷重软化温度。
在更低温度下形成烧胀陶粒,降低粉煤灰陶粒烧成温度10%以上。稀土氧化物与粉煤灰高温反应过程中的低熔点液相具备一定黏度,会优先包覆在陶粒表面,通过塑性变形方式锁住内部成气成分所产生的气体,并形成一个个密闭气孔。因此稀土氧化物的引入能降低烧胀陶粒的烧成温度。
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
一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,包括如下步骤:
(1)取粉煤灰经17K震荡分级,除去300微米以上漂珠,剩余筛分粉煤灰进行800℃高温焙烧5h后出料空冷至25℃经高能气流磨研磨,研磨后取1200目筛下料1940g,粉煤灰成分为氧化铝26%、氧化硅45%、氧化钙11%、氧化镁3%、氧化铁6.05%、钾钠1.25%;
(2)氧化镧铈(REO=99.56%)配比成50%固含量进入球磨机高能研磨,线速度8m/s,出料温度25℃,研磨至D90=500nm时进行喷雾干燥处理,进料速度2L/min,热喷温度270℃,干燥后D90粒径为2μm的微粉,取喷雾干燥后氧化镧铈60g,将氧化镧铈与粉煤灰在三维混粉机充分混合1h,得到混合粉体;
(3)将混合粉体装入造粒机,盘面倾斜35°,设定转速20rpm,均匀滴入中性水200g,待陶粒直径d=15mm左右出料,温度25℃,湿度45%处陈化14h,陈化后陶粒装入马弗炉,10℃/min升温至200℃,200℃保温30min后,以5℃/min升温至1250℃,保温20min,可得到氧化镧铈改性粉煤灰烧胀陶粒。
实施例2
一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,包括如下步骤:
(1)取粉煤灰经17K震荡分级,除去300微米以上漂珠,剩余筛分粉煤灰进行800℃高温焙烧5h后出料空冷至25℃经高能气流磨研磨,研磨后取1200目筛下料1900g,粉煤灰成分为氧化铝26%、氧化硅45%、氧化钙11%、氧化镁3%、氧化铁6.05%、钾钠2.25%;
(2)将氧化镧(99.5%)与氧化钐(99.5%)分别进入球磨机高能研磨,线速度8m/s,出料温度25℃,研磨至D90=500nm时进行喷雾干燥处理,进料速度2L/min,热喷温度270℃,干燥后D90粒径为2μm的微粉,将氧化镧70g、氧化钐30g与粉煤灰在三维混粉机充分混合1h,得到混合粉体;
(3)将混合粉体装入造粒机,盘面倾斜35°,设定转速20rpm,均匀滴入水玻璃(10%)200g,待陶粒直径d=15mm左右出料,温度25℃,湿度45%处陈化14h,陈化后陶粒装入马弗炉,10℃/min升温至200℃,200℃保温30min后,以5℃/min升温至1190℃,保温20min,可得到氧化镧氧化钐改性粉煤灰烧胀陶粒。
实施例3
一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,包括如下步骤:
(1)取粉煤灰经17K震荡分级,除去300微米以上漂珠,剩余筛分粉煤灰进行800℃高温焙烧5h后出料空冷至25℃经高能气流磨研磨,研磨后取1200目筛下料1900g,粉煤灰成分为氧化铝26%、氧化硅45%、氧化钙11%、氧化镁3%、氧化铁6.05%、钾钠2.25%;
(2)将氧化镧(3N)与氧化钇(3N)分别进入球磨机高能研磨,线速度8m/s,出料温度25℃,研磨至D90=500nm时进行喷雾干燥处理,进料速度2L/min,热喷温度270℃,干燥后D90粒径为2μm的微粉,将氧化镧110g、氧化钇30g与粉煤灰在三维混粉机充分混合1h,得到混合粉体;
(3)将混合粉体装入造粒机,盘面倾斜35°,设定转速20rpm,均匀滴入磷酸二氢铝溶液(5%)200g,待陶粒直径d=15mm左右出料,温度25℃,湿度45%处陈化14h,陈化后陶粒装入马弗炉,10℃/min升温至200℃,200℃保温30min后,以5℃/min升温至1170℃,保温20min,可得到氧化镧氧化钇改性粉煤灰烧胀陶粒。
对比例1
一种粉煤灰陶粒的制备方法,包括如下步骤:
(1)取粉煤灰经17K震荡分级,除去300微米以上漂珠,剩余筛分粉煤灰进行800℃高温焙烧5h后出料空冷至25℃经高能气流磨研磨,研磨后取1200目筛下料1940g,粉煤灰成分为氧化铝26%、氧化硅45%、氧化钙11%、氧化镁3%、氧化铁6.05%、钾钠1.25%;
(2)将混合粉体装入造粒机,盘面倾斜35°,设定转速20rpm,均匀滴入中性水200g,待陶粒直径d=15mm左右出料,温度25℃,湿度45%处陈化14h,陈化后陶粒装入马弗炉,10℃/min升温至200℃,200℃保温30min后,以5℃/min升温至1250℃,保温20min,可得到粉煤灰烧胀陶粒。
对比例2
一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,包括如下步骤:
(1)取粉煤灰1940g,粉煤灰成分为氧化铝22%、氧化硅53%、氧化钙9%、氧化镁2.3%、氧化铁4.95%、钾钠3.35%;
(2)氧化镧铈(REO=99.56%)配比成50%固含量进入球磨机高能研磨,线速度8m/s,出料温度25℃,研磨至D90=500nm时进行喷雾干燥处理,进料速度2L/min,热喷温度270℃,干燥后D90粒径为2μm的微粉,取喷雾干燥后氧化镧铈60g,将氧化镧铈与粉煤灰在三维混粉机充分混合1h,得到混合粉体;
(3)将混合粉体装入造粒机,盘面倾斜35°,设定转速20rpm,均匀滴入中性水200g,待陶粒直径d=15mm左右出料,温度25℃,湿度45%处陈化14h,陈化后陶粒装入马弗炉,10℃/min升温至200℃,200℃保温30min后,以5℃/min升温至1250℃,保温20min,产物含有低熔点玻璃微珠,陶粒1250℃焙烧后熔融液化,无法保持球型。
对比例3
一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,包括如下步骤:
(1)取粉煤灰经17K震荡分级,除去300微米以上漂珠,剩余筛分粉煤灰进行800℃高温焙烧5h后出料空冷至25℃后取料1940g,粉煤灰成分为氧化铝26%、氧化硅45%、氧化钙11%、氧化镁3%、氧化铁6.05%、钾钠1.25%;
(2)氧化镧铈(REO=99.56%)配比成50%固含量进入球磨机高能研磨,线速度8m/s,出料温度25℃,研磨至D90=500nm时进行喷雾干燥处理,进料速度2L/min,热喷温度270℃,干燥后D90粒径为2μm的微粉,取喷雾干燥后氧化镧铈60g,将氧化镧铈与粉煤灰在三维混粉机充分混合1h,得到混合粉体;
(3)将混合粉体装入造粒机,盘面倾斜35°,设定转速20rpm,均匀滴入中性水200g,待陶粒直径d=15mm左右出料,温度25℃,湿度45%处陈化14h,陈化后陶粒装入马弗炉,10℃/min升温至200℃,200℃保温30min后,以5℃/min升温至1250℃,保温20min,可得到氧化镧铈改性粉煤灰烧胀陶粒,氧化镧铈粉煤灰混合粉体材料围观组成不够均匀,烧胀气孔分布不均且容易造成气孔分布在陶粒表层,陶粒芯层无气孔产生。
对各实施例与各对比例的陶粒产物进行性能测试,结果如表1所示。
表1性能数据表
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:包括如下步骤:
步骤1是粉煤灰的前处理:将粉煤灰进行震荡、高温焙烧、研磨、过筛后得到;
步骤2是陶粒的制备:将稀土氧化物进行球磨、喷雾干燥后与所述的粉煤灰粉体进行共混后得到混合粉体;
步骤3是成球工艺:将所述的混合粉体置于造粒机中,将粘结剂均匀滴加入所述的混合粉体中,然后将制得的陶粒进行陈化、焙烧后得到所述的稀土氧化物粉煤灰陶粒。
2.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤2中的稀土氧化物为氧化镧、氧化铈、氧化钐、氧化钇、氧化镧铈或氧化镧钐中的至少一种;所述的步骤2中的稀土氧化物的纯度REO≥98%;所述的步骤2中的稀土氧化物的固含量为25-80%。
3.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤2中的球磨步骤的线速度为1-13m/s,温度为15-40℃,研磨后的料浆的粒径为500nm≤D90≤1000nm;所述的步骤2中的喷雾干燥步骤的进料速度为0.1-60L/min,温度为210-280℃,喷雾干燥后的粉体的粒径为1μm≤D90≤5μm。
4.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤2中经喷雾干燥后的稀土氧化物粉体与所述的粉煤灰粉体的质量比为1-12:88-99。
5.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤3中的粘结剂为水、水玻璃、磷酸二氢铝、硅溶胶、铝溶胶或锆溶胶中的至少一种;所述的步骤3中的粘结剂与所述的混合粉体的质量比为15-28:72-85。
6.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤3中的造粒机的倾斜角为30°-50°,转速为10-60rpm;所述的步骤3的滴加步骤的速率为0.0001-10L/s;所述的步骤3中的陶粒的直径为1.5-15mm。
7.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤3中的陈化步骤的温度为18-30℃,湿度为35-65%,时间为8-24h。
8.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤3中的焙烧步骤的参数如下:以5-30℃/min的速率由室温升温至200℃,200℃保温15-300min,以3-10℃/min的速率由200℃升温至1100-1350℃,保温1-150min后冷却至室温。
9.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤1中的震荡步骤的分级为17-28K,筛分出300μm以上的漂珠;所述的步骤1中的高温焙烧步骤的温度为750-900℃,时间为1-5h;所述的步骤1中的研磨步骤过1200目筛网后的筛余率≤5%。
10.根据权利要求1所述的高荷重软化温度的稀土氧化物粉煤灰陶粒的制备方法,其特征在于:所述的步骤1中的粉煤灰由包括如下质量百分比的组分组成:氧化铝10-45%,氧化硅25-55%,氧化钙≤15%,氧化镁≤5%,氧化铁≤7%,钾钠≤5%。
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