CN113651633B - 一种莫来石纤维增强碳化硅陶瓷过滤管及其制备方法 - Google Patents
一种莫来石纤维增强碳化硅陶瓷过滤管及其制备方法 Download PDFInfo
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- CN113651633B CN113651633B CN202110847971.XA CN202110847971A CN113651633B CN 113651633 B CN113651633 B CN 113651633B CN 202110847971 A CN202110847971 A CN 202110847971A CN 113651633 B CN113651633 B CN 113651633B
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- silicon carbide
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- ceramic filter
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 205
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 146
- 239000000919 ceramic Substances 0.000 title claims abstract description 112
- 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 84
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 84
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- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 16
- 239000005995 Aluminium silicate Substances 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
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- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 14
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 12
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- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 7
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 7
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种莫来石纤维增强碳化硅陶瓷过滤管及其制备方法，该过滤管在碳化硅陶瓷支撑体及表面膜层之间设有一层莫来石纤维过渡层，其制备方法如下：1)将混合碳化硅粉体、粘接剂、造孔剂、分散剂、无水乙醇和去离子水称取备用；2)将粘结剂与去离子水混合得到粘结剂浆料；3)将分散剂与无水乙醇混合得到分散剂溶液，与混合碳化硅粉体混合均匀得到碳化硅浆料；4)将一部分粘接剂浆料喷涂到支撑体表面，剩余粘接剂浆料加入碳化硅浆料中，再加入造孔剂，将所得浆料采用流延法在碳化硅陶瓷支撑体外表面涂膜，烘干再烧结得到莫来石纤维增强碳化硅陶瓷过滤管。本发明提供的莫来石纤维增强碳化硅陶瓷过滤管具有强度高、耐高温、耐腐蚀等优点。
Description
技术领域
本发明属于采用刚性空心滤体的粒子分离器技术领域，涉及一种莫来石纤维增强碳化硅陶瓷过滤管及其制备方法。
背景技术
近年以来，随着我国城市的工业化和城市化建设的高速发展，环境能源的消耗量也在迅速增加。煤炭目前仍然处于主体能源地位，是我国基础能源和重要的工业原料，由于煤炭在利用中会产生大量成分复杂有害的高温废气，直接排放会导致水污染和大气污染问题，因此，废气需要进行严格处理减少环境污染。
利用无机陶瓷过滤管对废气进行过滤处理的方法具有效率高、能耗低和环境友好等一系列优势，其中碳化硅陶瓷由于具有耐高温、耐腐蚀、抗热冲击、亲水性强以及使用寿命长等突出优点，可应用在各种恶劣的环境条件下，从而得到广泛应用。目前常见的多孔碳化硅陶瓷过滤管的结构包括位于过滤管内层提供力学强度的支撑体及附着在支撑体外面的除去粉尘等污染物颗粒的表面膜层，采用两层结构用于粉尘等污染物的吸附。但在多孔碳化硅陶瓷过滤管制备成型过程中，表面膜层的粉料会进入支撑体孔隙中，使表面膜实际厚度大于名义厚度，一定程度上提高了过滤压，不仅会降低过滤精度和过滤效率，甚至影响其使用寿命。
发明内容
本发明所要解决的技术问题是针对现有技术中存在的上述不足，提供一种莫来石纤维增强碳化硅陶瓷过滤管及其制备方法，在原有支撑体和表面膜层之间增加一层莫来石纤维过渡层，不仅能使表面膜成膜更均匀，还能防止表面膜粉料进入支撑体孔隙，降低过滤压，同时具有很高的机械强度和耐酸碱性等优异性能。
为解决上述技术问题，本发明提供的技术方案是：
提供一种莫来石纤维增强碳化硅陶瓷过滤管，所述莫来石纤维增强碳化硅陶瓷过滤管在碳化硅陶瓷支撑体及表面膜层之间设有一层莫来石纤维过渡层，其制备方法包括以下步骤：
1)将混合碳化硅粉体、粘接剂、造孔剂、分散剂、无水乙醇和去离子水按以下质量百分比称取，备用：混合碳化硅粉体49～63％，粘接剂6.5～15％，造孔剂0.25～1％，分散剂1.4～3.4％，去离子水6～13％，无水乙醇17.9～21.6％；
2)将粘结剂与去离子水混合，得到粘结剂浆料；
3)将分散剂与无水乙醇混合，得到分散剂溶液，将分散剂溶液与混合碳化硅粉体混合均匀得到碳化硅浆料；
4)将一部分步骤2)制备的粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，将剩余的粘接剂浆料少量多次地加入到步骤3)所制备的碳化硅浆料中，再加入造孔剂，搅拌均匀得到浆料，将所得浆料采用流延法在碳化硅陶瓷支撑体外表面涂膜，得到碳化硅陶瓷过滤管半成品，然后将整个碳化硅陶瓷过滤管半成品烘干，再移入烧结炉中烧结，得到莫来石纤维增强碳化硅陶瓷过滤管。
按上述方案，所述莫来石纤维过渡层厚度为20～50μm。
按上述方案，步骤1)所述混合碳化硅粉体由粗碳化硅粉体与细碳化硅粉体按质量份比85～90：10～15混合得到，两者合计100份，其中粗碳化硅粉体的粒径D50为20～60μm，细碳化硅粉体的粒径D50为10～20μm，粗碳化硅粉体与细碳化硅粉体的纯度均为98wt％以上。采用不同粒径的碳化硅粉体，在高温重结晶过程中，较小的碳化硅颗粒先升华后凝结，大颗粒晶体长大，最终形成具有高结合强度的立体连通结构，可进一步提升所得碳化硅陶瓷支撑体的抗折强度、纯度以及耐腐蚀性。
按上述方案，步骤1)所述粘接剂由钾长石粉体、石英砂和高岭土粉体按照质量比60～68：8～16：19～32混合得到，所述钾长石粉体粒径为15～30μm，其中K2O含量8～15wt％，Al2O3含量17～20wt％，SiO2含量62～74wt％；所述石英砂目数为200目以上，SiO2含量≥95％；所述高岭土粉体粒径10～20μm，Al2O3含量40～46wt％，SiO2含量46～50wt％。根据K2O-SiO2-Al2O3相图通过固相反应生成莫来石。其次钾长石的熔融温度为1200℃左右，在烧结过程中会形成液相，会包覆颗粒与之结合，是一种合适的助溶剂。在钾长石的助溶作用下，高岭土首先在500～900℃转变成铝活性较高的偏高岭土，其所提供的铝源能与细度较小的石英开始反应促进莫来石相的生成；继续升温至1000℃左右，开始有非晶莫来石相和玻璃相出现，此时非晶莫来石相与碳化硅颗粒有较好的化学相容性，能够伴随着玻璃相流动，意味着在支撑体和粘接剂层会有莫来石相互相渗透，形成具有莫来石纤维增强的过度膜层；到1200℃，钾长石既能作为烧结助剂熔融，使部分莫来石液相能够与碳化硅颗粒粘接在一起，而且它能提供钾源，抑制方石英相的生成。降温时液相的莫来石凝固，将整体结构紧密结合在一起。所用石英细度很小，表面活性高较高，可以在烧结开始阶段加速反应进行。
按上述方案，步骤1)所述造孔剂为炭黑，粒径为1.5μm。
按上述方案，步骤1)所述分散剂由甲基纤维素、四甲基氢氧化铵和羧甲基纤维素钠按质量比1：1～2：0.9～1.3复配得到。选用这三种原料复配能使得体系处于一个高度稳定的分散状态，避免出现粉体颗粒之间吸附聚集而形成大颗粒沉降的现象。
按上述方案，步骤2)所述粘结剂浆料固含量为40～60wt％。
按上述方案，步骤4)粘接剂浆料喷涂到碳化硅陶瓷支撑体表面的厚度为10～25μm。
按上述方案，步骤4)采用流延法在碳化硅陶瓷支撑体外表面涂膜厚度为0.1～1mm。
按上述方案，步骤4)所述烘干条件为：105℃下烘3h。
按上述方案，步骤4)所述烧结工艺条件为：在埋炭气氛下，从室温下以5℃/min的速率升温到550℃，保温1～2h，然后以490～510mL/min的流速通入氩气洗炉，洗炉时间为20min，接着再以5℃/min的速率升温至1280℃，保温2～3h，随后以2℃/min的速率升温至1560℃，保温80～90min，最后以5℃/min的速率降温至300～400℃，保温30～60min，并随炉自然冷却至室温。碳化硅在高温下与氧气可以生成二氧化硅，附着在碳化硅表面，冷却时虽可将碳化硅颗粒粘接在一起使样品增加一定强度，但冷却后的样品由于附着二氧化硅，耐碱性差。在埋炭气氛中，既可以防止碳化硅被氧化，也能让粉料中的氧化铝和二氧化硅反应生成莫来石相。550℃左右是高岭土开始反应的温度区间，洗炉处理能够减少其他杂质气氛的影响。
本发明还包括上述莫来石纤维增强碳化硅陶瓷过滤管的制备方法，具体步骤如下：
1)将混合碳化硅粉体、粘接剂、造孔剂、分散剂、无水乙醇和去离子水按以下质量百分比称取，备用：混合碳化硅粉体49～63％，粘接剂6.5～15％，造孔剂0.25～1％，分散剂1.4～3.4％，去离子水6～13％，无水乙醇17.9～21.6％；
2)将粘结剂与去离子水混合，得到粘结剂浆料；
3)将分散剂与无水乙醇混合，得到分散剂溶液，将分散剂溶液与混合碳化硅粉体混合均匀得到碳化硅浆料；
4)将一部分步骤2)制备的粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，将剩余的粘接剂浆料少量多次地加入到步骤3)所制备的碳化硅浆料中，再加入造孔剂，搅拌均匀得到浆料，将所得浆料采用流延法在碳化硅陶瓷支撑体外表面涂膜，得到碳化硅陶瓷过滤管半成品，然后将整个碳化硅陶瓷过滤管半成品烘干，再移入烧结炉中烧结，得到莫来石纤维增强碳化硅陶瓷过滤管。
本发明还包括上述莫来石纤维增强碳化硅陶瓷过滤管在气体处理领域的应用。
本发明在碳化硅陶瓷支撑体与表面膜层之间形成了一层莫来石纤维过渡层。莫来石物相晶区不仅在高温下能与碳化硅形成良好表面浸润，而且熔融温度也远高于支撑体的使用温度。由于在支撑体表面直接涂覆过滤膜时，会有一部分膜料进入支撑体空隙内部，导致陶瓷颗粒过滤膜的过滤压降增大，而本发明引入莫来石纤维过渡层不仅能有效降低过滤压降，同时产生的莫来石纤维膜能够更好地吸附浆料，而且相互渗透的莫来石纤维能促进碳化硅陶瓷过滤管整体结构更稳定。而碳化硅陶瓷支撑体在这种类似于双层过滤膜层包覆的基础上，拥有了良好的微观性能和抗弯强度，同时因莫来石具有良好的高温强度，其热膨胀系数与碳化硅相近，有良好的化学兼容性，可以实现低温烧结，有效降低生产成本。
本发明的原理为：
1)本发明以K2O-SiO2-Al2O3相图为标准，控制钾长石、高岭土和石英的比例，在支撑体与表面膜层之间烧结莫来石纤维来增强碳化硅陶瓷管的结构，所生成的莫来石纤维和碳化硅有很好的化学相容性，结构稳定，环境友好；粘接剂首先在支撑体上涂覆一层，有助于在烧结过程中连接过度膜层中的莫来石相；而钾长石作为烧结助剂，在高岭土的烧结中，为其提供了液相的烧结环境，使不同位置的莫来石相能够相互渗透在一起，而且还提供了钾源，抑制方石英的生成。
2)本发明在碳化硅陶瓷支撑体与表面膜层之间形成了一层莫来石纤维的过渡层，能够防止一部分膜料进入支撑体空隙内部引起的陶瓷颗粒过滤膜的过滤压降增大。而莫来石纤维层不仅能有效降低压降，同时产生的纤维膜能够更好的吸附浆料。
本发明的有益效果在于：1、本发明提供的莫来石纤维增强碳化硅陶瓷过滤管具有强度高、耐高温、耐腐蚀等优异特点，所形成的莫来石纤维层不仅能有效降低压降，同时产生的纤维膜能够更好地吸附浆料。2、本发明提供的制备方法步骤简单、工艺控制灵活、煅烧温度低，明显降低了工艺成本，具有重要的推广价值，可大规模应用。
附图说明
图1为本发明实施例1所制备的莫来石纤维增强碳化硅陶瓷过滤管表面SEM图；
图2为实施例1所制备的莫来石纤维增强碳化硅陶瓷过滤管断面SEM图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合实施例对本发明作进一步详细描述。
以下实施例中，所用碳化硅陶瓷支撑体为实验室统一烧制的碳化硅支撑体样品，其气孔率26～35％，抗弯强度18～26MPa；所用粗碳化硅粉体的粒度为D50＝30μm，细碳化硅粉体的粒度为D50＝10μm，两种粒径的碳化硅粉体的纯度为98wt％以上；所用钾长石粉体平均粒径为16μm，其中K2O含量12wt％，Al2O3含量17wt％，SiO2含量65wt％；所述石英砂目数为200目，SiO2含量≥95％；所述高岭土粉体平均粒径10μm，Al2O3含量45wt％，SiO2含量49wt％；所用造孔剂为炭黑，粒径为1.5μm。
实施例1
一种莫来石纤维增强碳化硅陶瓷过滤管，其制备方法包括以下步骤：
1)将粗碳化硅粉体和细碳化硅粉体按质量比90：10混合搅拌均匀，得到混合碳化硅粉体，备用；将甲基纤维素、四甲基氢氧化铵、羧甲基纤维素钠按照质量比1：1：0.9混合，得到分散剂；将钾长石粉体、石英砂和高岭土粉体按照质量比60：8：19混合得到粘接剂；
2)按以下质量百分配比称取各原料：混合碳化硅粉体63％、粘接剂6.5％、造孔剂0.3％、分散剂1.4％、去离子水10％、无水乙醇18.8％；
3)将粘接剂与去离子水混合，制得粘接剂浆料；将分散剂与无水乙醇混合，制得分散剂溶液，将分散剂溶液与混合碳化硅粉体搅拌混合均匀，得碳化硅浆料；
4)将一部分粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，喷涂厚度为10μm，将剩余的粘接剂浆料少量多次地加入到碳化硅浆料中，使粘接剂包裹在碳化硅骨料表面，再加入造孔剂，搅拌3min，得到浆料；
5)把步骤4)所得浆料采用流延法在碳化硅陶瓷支撑体外表面制备成表面膜层，膜层厚度为0.2mm，得到碳化硅陶瓷过滤管半成品，将半成品在105℃温度下干燥3h后转移至高温炉中，在埋炭气氛中从室温下以5℃/min的速率升温到550℃，保温1h，再以500mL/min的流速通入氩气进行洗炉，洗炉时间为20min，接着再以5℃/min的速率升温至1280℃，保温2h，然后以2℃/min的速率升温至1560℃，保温90min，最后以5℃/min的速率降温至300℃，保温45min，并随炉自然冷却至室温，即得莫来石纤维增强碳化硅陶瓷过滤管。
本实施例制备的莫来石纤维增强碳化硅陶瓷过滤管，整个过滤管内部气孔均匀，且孔径差别不大，气孔率33％，抗弯强度达34Mpa，在碳化硅陶瓷支撑体及表面膜层之间生成一层莫来石纤维过渡层，厚度为26μm。在进气侧压力为0.1MPa的情况下，莫来石纤维增强碳化硅陶瓷过滤管过滤压降为855Pa，对PM1.0的含尘烟气的过滤度为96％。
图1所示为本实施例制备的莫来石纤维增强碳化硅陶瓷过滤管表面SEM图，图中可以看出碳化硅颗粒表面光滑，表现出良好的烧结性能。
图2所示为本实施例制备的莫来石纤维增强碳化硅陶瓷过滤管的断面SEM图，可以看出在碳化硅陶瓷支撑体及表面膜层之间生成一层莫来石纤维过渡层，并且莫来石纤维过渡层与碳化硅陶瓷支撑体充分接触。
实施例2
一种莫来石纤维增强碳化硅陶瓷过滤管，其制备方法包括以下步骤：
1)将粗碳化硅粉体和细碳化硅粉体按质量比85：15混合搅拌均匀，得到混合碳化硅粉体，备用；将甲基纤维素、四甲基氢氧化铵、羧甲基纤维素钠按照质量比1：2：1.3混合得到分散剂；将钾长石粉体、石英砂和高岭土粉体按照质量比68：16：27混合得到粘接剂；
2)按以下质量百分配比称取各原料：混合碳化硅粉体60％、粘接剂12％、造孔剂0.7％、分散剂2％、去离子水6％、无水乙醇19.3％；
3)将粘接剂与去离子水混合，制得粘接剂浆料；将分散剂与无水乙醇混合，制得分散剂溶液，将分散剂溶液与混合碳化硅粉体搅拌混合均匀，得碳化硅浆料；
4)将一部分粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，喷涂厚度为18μm；将剩余的粘接剂浆料少量多次地加入到碳化硅浆料中，使粘接剂包裹在碳化硅骨料表面，再加入造孔剂，搅拌4min，得到浆料；
5)把步骤4)所得浆料采用流延法在碳化硅陶瓷支撑体外表面制备成表面膜层，厚度为0.5mm，得到碳化硅陶瓷过滤管半成品，然后将半成品在105℃温度下干燥3h后转移至高温炉中，在埋炭气氛中从室温下以5℃/min的速率升温到550℃，保温1h，再以490mL/min的流速通入氩气进行洗炉，洗炉时间为20min，接着再以5℃/min的速率升温至1280℃，保温2h，然后以2℃/min的速率升温至1560℃，保温90min，最后以5℃/min的速率降温至300℃，保温40min，并随炉自然冷却至室温，即得莫来石纤维增强碳化硅陶瓷过滤管。
本实施例制备的莫来石纤维增强碳化硅陶瓷过滤管整个过滤管内部气孔均匀，且孔径差别不大，气孔率26％，抗弯强度达41Mpa，在碳化硅陶瓷支撑体及表面膜层之间生成一层莫来石纤维过渡层，厚度为34μm。在进气侧压力为0.1MPa的情况下，莫来石纤维增强碳化硅陶瓷过滤管过滤压降为785Pa，对PM1.0的含尘烟气的过滤度为98％。
实施例3
一种莫来石纤维增强碳化硅陶瓷过滤管，其制备方法包括以下步骤：
1)将粗碳化硅粉体和细碳化硅粉体按质量比88：12混合搅拌均匀，得到混合碳化硅粉体，备用；将甲基纤维素、四甲基氢氧化铵、羧甲基纤维素钠按照质量比1：1.5：1.1混合，得到分散剂；将钾长石粉体、石英砂和高岭土粉体按照质量比64：12：23混合得到粘接剂粉料；
2)按以下质量百分配比称取各原料：混合碳化硅粉体55％、粘接剂10％、造孔剂0.6％、分散剂2.8％、去离子水10％、无水乙醇21.6％；
3)将粘接剂与去离子水混合，制得粘接剂浆料；将分散剂与无水乙醇混合，制得分散剂溶液，将分散剂溶液与混合碳化硅粉体搅拌混合均匀，得碳化硅浆料；
4)将一部分粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，喷涂厚度为20μm；将剩余的粘接剂浆料少量多次地加入到碳化硅浆料中，使粘接剂包裹在碳化硅骨料表面，再加入造孔剂，搅拌5min，得到浆料；
5)把步骤4)所得浆料采用流延法在碳化硅陶瓷支撑体外表面制备成表面膜层，厚度为0.8mm，得到碳化硅陶瓷过滤管半成品，然后将半成品在105℃温度下干燥3h后转移至高温炉中，在埋炭气氛中从室温下以5℃/min的速率升温到550℃，保温1h，再以510mL/min的流速通入氩气进行洗炉，洗炉时间为20min，接着再以5℃/min的速率升温至1280℃，保温2h，然后以2℃/min的速率升温至1560℃，保温90min，最后以5℃/min的速率降温至360℃，保温38min，并随炉自然冷却至室温，即得莫来石纤维增强碳化硅陶瓷过滤管。
本实施例制备的莫来石纤维增强碳化硅陶瓷过滤管整个过滤管内部气孔均匀，且孔径差别不大，气孔率22％，抗弯强度达46Mpa，在碳化硅陶瓷支撑体及表面膜层之间生成一层莫来石纤维过渡层，厚度为38μm。在进气侧压力为0.1MPa的情况下，莫来石纤维增强碳化硅陶瓷过滤管过滤压降为763Pa，对PM1.0的含尘烟气的过滤度为97％。
实施例4
一种莫来石纤维增强碳化硅陶瓷过滤管，其制备方法包括以下步骤：
1)粗碳化硅粉体和细碳化硅粉体按质量比89：11混合搅拌均匀，得到混合碳化硅粉体，备用；将甲基纤维素、四甲基氢氧化铵、羧甲基纤维素钠按照质量比1：1.2：1.1混合，得到分散剂；将钾长石粉体、石英砂和高岭土粉体按照质量比66：14：25混合得到粘接剂；
2)按以下质量百分配比称取各原料：混合碳化硅粉体52％、粘接剂14％、造孔剂0.3％、分散剂2.5％、去离子水12％、无水乙醇19.2％；
3)将粘接剂与去离子水混合，制得粘接剂浆料；将分散剂与无水乙醇混合，制得分散剂溶液，将分散剂溶液与混合碳化硅粉体搅拌混合均匀，得碳化硅浆料；
4)将一部分粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，喷涂厚度为13μm，将剩余的粘接剂浆料少量多次地加入到碳化硅浆料中，使粘接剂包裹在碳化硅骨料表面，再加入将造孔剂，搅拌3min，得到浆料；
5)把步骤4)所得浆料采用流延法在碳化硅陶瓷支撑体外表面制备成表面膜层，厚度为0.5mm，得到莫来石纤维增强碳化硅陶瓷过滤管半成品，然后将半成品在105℃下干燥3h后转移至高温炉中，在埋炭气氛中从室温下以5℃/min的速率升温到550℃，保温1h，再以510mL/min的流速通入氩气进行洗炉，洗炉时间为20min，接着再以5℃/min的速率升温至1280℃，保温2h，然后以2℃/min的速率升温至1560℃，保温80min，最后以5℃/min的速率降温至360℃，保温38min，并随炉自然冷却至室温，即得莫来石纤维增强碳化硅陶瓷过滤管。
本实施例制备的莫来石纤维增强碳化硅陶瓷过滤管整个过滤管内部气孔均匀，且孔径差别不大，气孔率27％，抗弯强度达36Mpa，在碳化硅陶瓷支撑体及表面膜层之间生成一层莫来石纤维过渡层，厚度为28μm。在进气侧压力为0.1MPa的情况下，莫来石纤维增强碳化硅陶瓷过滤管过滤压降为1030Pa，对PM1.0的含尘烟气的过滤度为95％。
实施例5
一种莫来石纤维增强碳化硅陶瓷过滤管，其制备方法包括以下步骤：
1)粗碳化硅粉体和细碳化硅粉体按质量比84：16混合搅拌均匀，得到混合碳化硅粉体，备用；将甲基纤维素、四甲基氢氧化铵、羧甲基纤维素钠按照1：1.8：1的质量比混合，得到分散剂；将钾长石粉体、石英砂和高岭土粉体按照质量比63：11：22混合得到粘接剂；
2)按以下质量百分配比称取各原料：混合碳化硅粉体57％、粘接剂9％、造孔剂0.8％、分散剂2.3％、去离子水13％、无水乙醇17.9％；
3)将粘接剂与去离子水混合，制得粘接剂浆料；将分散剂与无水乙醇混合，制得分散剂溶液，将分散剂溶液与混合碳化硅粉体搅拌混合均匀，得碳化硅浆料；
4)将一部分粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，喷涂厚度为15μm；将剩余的粘接剂浆料少量多次地加入到碳化硅浆料中，使粘接剂包裹在碳化硅骨料表面，再加入造孔剂，搅拌5min，得到浆料；
5)把步骤4)所得浆料采用流延法在碳化硅陶瓷支撑体外表面制备成表面膜层，厚度为0.5mm，得到莫来石纤维增强碳化硅陶瓷过滤管半成品，然后将半成品在105℃温度下干燥3h后转移至高温炉中，在埋炭气氛中从室温下以5℃/min的速率升温到550℃，保温1h，再以510mL/min的流速通入氩气进行洗炉，洗炉时间为20min，接着再以5℃/min的速率升温至1280℃，保温2h，然后以2℃/min将速率升到1560℃，保温80min，最后以5℃/min的速率降温至360℃，保温38min，并随炉自然冷却至室温，即得莫来石纤维增强碳化硅陶瓷过滤管。
本实施例制备的莫来石纤维增强碳化硅陶瓷过滤管整个过滤管内部气孔均匀，且孔径差别不大，气孔率28％，抗弯强度达38Mpa，在碳化硅陶瓷支撑体及表面膜层之间生成一层莫来石纤维过渡层，厚度为31μm。在进气侧压力为0.1MPa的情况下，莫来石纤维增强碳化硅陶瓷过滤管过滤压降为810Pa，对PM1.0的含尘烟气的过滤度为95％。
对比例1
一种碳化硅陶瓷过滤管的制备方法，其具体步骤与实施例1相似，不同之处在于没有在支撑体表面涂覆一层粘接剂浆料。
通过对所制得的过滤管成品进行测试，气孔率为27％，抗弯强度为22Mpa；在进气侧压力为0.1MPa的情况下，过滤压降为1580Pa；对PM1.0的含尘烟气过滤度为92％。
对比例2
一种碳化硅陶瓷过滤管的制备方法，其具体步骤与实施例2相似，不同之处在于没有在支撑体表面涂覆一层粘接剂浆料。
通过对所制得的过滤管成品进行测试，气孔率为22％，抗弯强度为31Mpa；在进气侧压力为0.1MPa的情况下，过滤压降为1350Pa；对PM1.0的含尘烟气过滤度为93％。
Claims (8)
1.一种莫来石纤维增强碳化硅陶瓷过滤管，其特征在于，所述莫来石纤维增强碳化硅陶瓷过滤管在碳化硅陶瓷支撑体及表面膜层之间设有一层莫来石纤维过渡层，其制备方法包括以下步骤：
1）将混合碳化硅粉体、粘接剂、造孔剂、分散剂、无水乙醇和去离子水按以下质量百分比称取，备用：混合碳化硅粉体49~63%，粘接剂6.5~15%，造孔剂0.25~1%，分散剂1.4~3.4%，去离子水6~13%，无水乙醇17.9~21.6%，所述混合碳化硅粉体由粗碳化硅粉体与细碳化硅粉体按质量份比85~90：10~15混合得到，两者合计100份，其中粗碳化硅粉体的粒径D50为20~60μm，细碳化硅粉体的粒径D50为10~20μm，粗碳化硅粉体与细碳化硅粉体的纯度均为98wt%以上，所述粘接剂由钾长石粉体、石英砂和高岭土粉体按照质量比60~68：8~16：19~32混合得到，所述钾长石粉体粒径为15~30μm，其中K2O含量8~15wt%，Al2O3含量17~20wt%，SiO2含量62~74wt%；所述石英砂目数为200目以上，SiO2含量≥95%；所述高岭土粉体粒径10~20μm，Al2O3含量40~46wt%，SiO2含量46~50wt%，所述分散剂由甲基纤维素、四甲基氢氧化铵和羧甲基纤维素钠按质量比1：1~2：0.9~1.3复配得到；
2）将粘结剂与去离子水混合，得到粘结剂浆料；
3）将分散剂与无水乙醇混合，得到分散剂溶液，将分散剂溶液与混合碳化硅粉体混合均匀得到碳化硅浆料；
4）将一部分步骤2）制备的粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，将剩余的粘接剂浆料少量多次地加入到步骤3）所制备的碳化硅浆料中，再加入造孔剂，搅拌均匀得到浆料，将所得浆料采用流延法在碳化硅陶瓷支撑体外表面涂膜，得到碳化硅陶瓷过滤管半成品，然后将整个碳化硅陶瓷过滤管半成品烘干，再移入烧结炉中烧结，所述烧结工艺条件为：在埋炭气氛下，从室温下以5℃/min的速率升温到550℃，保温1~2h，然后以490~510mL/min的流速通入氩气洗炉，洗炉时间为20min，接着再以5℃/min的速率升温至1280℃，保温2~3h，随后以2℃/min的速率升温至1560℃，保温80~90min，最后以5℃/min的速率降温至300~400℃，保温30~60min，并随炉自然冷却至室温，得到莫来石纤维增强碳化硅陶瓷过滤管。
2.根据权利要求1所述的莫来石纤维增强碳化硅陶瓷过滤管，其特征在于，所述莫来石纤维过渡层厚度为20~50μm。
3.根据权利要求1所述的莫来石纤维增强碳化硅陶瓷过滤管，其特征在于，步骤1）所述造孔剂为炭黑，粒径为1.5μm。
4.根据权利要求1所述的莫来石纤维增强碳化硅陶瓷过滤管，其特征在于，步骤2）所述粘结剂浆料固含量为40~60wt%。
5.根据权利要求1所述的莫来石纤维增强碳化硅陶瓷过滤管，其特征在于，步骤4）粘接剂浆料喷涂到碳化硅陶瓷支撑体表面的厚度为10~25μm；采用流延法在碳化硅陶瓷支撑体外表面涂膜厚度为0.1~1mm。
6.根据权利要求1所述的莫来石纤维增强碳化硅陶瓷过滤管，其特征在于，步骤4）所述烘干条件为：105℃下烘3h。
7.一种权利要求1-6任一所述的莫来石纤维增强碳化硅陶瓷过滤管的制备方法，其特征在于，具体步骤如下：
1）将混合碳化硅粉体、粘接剂、造孔剂、分散剂、无水乙醇和去离子水按以下质量百分比称取，备用：混合碳化硅粉体49~63%，粘接剂6.5~15%，造孔剂0.25~1%，分散剂1.4~3.4%，去离子水6~13%，无水乙醇17.9~21.6%；
2）将粘结剂与去离子水混合，得到粘结剂浆料；
3）将分散剂与无水乙醇混合，得到分散剂溶液，将分散剂溶液与混合碳化硅粉体混合均匀得到碳化硅浆料；
4）将一部分步骤2）制备的粘接剂浆料喷涂到碳化硅陶瓷支撑体表面，将剩余的粘接剂浆料少量多次地加入到步骤3）所制备的碳化硅浆料中，再加入造孔剂，搅拌均匀得到浆料，将所得浆料采用流延法在碳化硅陶瓷支撑体外表面涂膜，得到碳化硅陶瓷过滤管半成品，然后将整个碳化硅陶瓷过滤管半成品烘干，再移入烧结炉中烧结，得到莫来石纤维增强碳化硅陶瓷过滤管。
8.一种权利要求1-6任一所述的莫来石纤维增强碳化硅陶瓷过滤管在气体处理领域的应用。
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| CN1236840C (zh) * | 2001-06-08 | 2006-01-18 | 高斌 | 微孔陶瓷过滤板及制备方法 |
| CN1714909B (zh) * | 2005-05-11 | 2010-11-17 | 青海大学 | 洁净高温气体用陶瓷过滤管制备方法 |
| CN101607158B (zh) * | 2008-06-21 | 2011-06-15 | 淄博鑫拓耐火材料有限公司 | 碳化硅多孔陶瓷过滤器及其制造方法 |
| DE102011109682A1 (de) * | 2011-08-08 | 2013-02-14 | Technische Universität Bergakademie Freiberg | Verfahren zur Herstellung kohlenstoffhaltiger und/oder kohlenstoffgebundener keramischer Metallschmelze-Filter |
| CN102557730B (zh) * | 2011-12-13 | 2013-05-08 | 长安大学 | 一种碳化硅陶瓷表面改性方法 |
| CN102718494B (zh) * | 2012-06-21 | 2014-03-19 | 海南大学 | 一种复合碳化硅陶瓷过滤膜材料的制备方法 |
| CN103113110B (zh) * | 2012-12-04 | 2014-07-09 | 海南大学 | 一种复合碳化硅陶瓷纤维过渡层的涂覆方法 |
| CN103111132B (zh) * | 2013-02-25 | 2014-12-24 | 中国石油大学(北京) | 高温气体过滤管的制作装置和制作方法 |
| JP6077484B2 (ja) * | 2014-03-26 | 2017-02-08 | 日本碍子株式会社 | ハニカム構造体 |
| CN104478437A (zh) * | 2014-11-21 | 2015-04-01 | 安徽盛运环保（集团）股份有限公司 | 一种制造陶瓷过滤膜的原料以及工艺 |
| CN106178976A (zh) * | 2016-06-28 | 2016-12-07 | 董超超 | 一种含有二氧化钛颗粒的过滤膜 |
| CN106187297A (zh) * | 2016-08-26 | 2016-12-07 | 天津梦龙新能源技术有限公司 | 一种复合碳化硅陶瓷过滤膜材料的制备方法 |
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