CN107162626A - 一种碳化硅多孔陶瓷过滤膜材料的制备方法 - Google Patents
一种碳化硅多孔陶瓷过滤膜材料的制备方法 Download PDFInfo
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 11
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- 238000004140 cleaning Methods 0.000 claims description 7
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Abstract
本发明属于环保材料技术领域，具体涉及一种碳化硅多孔陶瓷过滤膜材料的制备方法。本发明首先将碳化硅粉末及陶瓷粘结剂粉末分散于羧甲基纤维素钠溶液中，再将浆料流延于以冰晶石、氧化铝及碳纤维压制成的中间层材料表面，随后在氮气保护状态下烧结，并在高温下使冰晶石和氧化铝熔融电解，产生氧气，形成多孔的中间层，在冷却固化过程中，中间层将上层过滤膜及下层支撑体牢固连接，最终经醋酸溶液浸泡，溶解除去部分中间层电解产生的铝，丰富其空隙结构，降低所得过滤膜在使用过程中的压降，节约能耗，有效解决了传统碳化硅过孔陶瓷过滤膜在制备过程中，过滤膜浆料因颗粒易进入支撑体材料孔隙的问题。
Description
技术领域
本发明属于环保材料技术领域，具体涉及一种碳化硅多孔陶瓷过滤膜材料的制备方法。
背景技术
能源的利用主要是通过直接燃烧来获得，由于现有技术的制约导致燃烧不充分，不仅能源利用效率较低，还排放出大量粉尘，对环境污染严重。提高能源利用效率，减少粉尘排放是目前材料学的重要研究方向。陶瓷过滤管被广泛应用在高温气体除尘净化技术中，已成为材料、冶金、化工、电力等行业实现气固分离、节能环保的关键部件。传统的高强度耐高温陶瓷过滤管一般采用两部分的结构，即支撑体部分和过滤膜部分。支撑体采用大粒径陶瓷颗粒来制备，能为过滤管内层提供力学强度，组成过滤膜的陶瓷颗粒则较小，保证了整个过滤体有足够的过滤除尘效率和精度。传统的陶瓷过滤管材料，由于制备支撑体的陶瓷颗粒粒径较大、孔径大，远大于表面膜的颗粒粒径，在其表面上制膜时，因表面膜粉料进入支撑体的空隙中，从而增加了过滤管材料的过滤压降程度，增加了膜的厚度，影响过滤管材料的整体性能。
复合碳化硅陶瓷过滤膜材料，是在碳化硅表面膜和碳化硅陶瓷支撑体之间增加陶瓷纤维过渡层，来达到改进过滤管材料的结构和性能，该纤维层不仅阻止了表面膜粉料进入支撑体空隙，而且有效降低了过滤材料的过滤压降程度。而多孔陶瓷过滤膜一般通过浆料涂层法制备，如提拉法、喷涂法和流延成型法等，但是由于多孔陶瓷基材的孔较多，孔径较大，表面也不平整，直接在多孔陶瓷基材表面上涂层时，主要出现三个缺陷：一、由于基材的孔径较大且不均匀，膜层易脱落，导致过滤膜浆料会进入基材空气中，影响其过滤效果。二、由于基材较多和表面不平整，不能提供有利于涂层时所有的光滑平整的表面，导致涂制的膜结构不光滑平整；三、多孔陶瓷过滤膜一般是先把多孔陶瓷基材压制成型后进行烧结，然后在基材上涂层，最后再烧结，其制备工艺复杂，且耗时长、耗能大，并且在实际的施工中抗化学侵蚀能力以及抗热震性都不好。因此，研究开发一种不易与支撑体脱离，且过滤效果极佳的陶瓷过滤膜材料具有重要的现实意义。
发明内容
本发明所要解决的技术问题是：针对传统碳化硅多孔陶瓷过滤膜材料在制备过程中，过滤膜浆料因颗粒易进入支撑体材料孔隙中，导致过滤膜过滤效果不佳的问题，提供了一种碳化硅多孔陶瓷过滤膜材料的制备方法。
为解决上述技术问题，本发明采用如下所述的技术方案：
（1）依次称取100～120g高岭土，200～220g石英石，600～650g钾长石，倒入球磨机中，按球料质量比为10：1～20：1加入氧化锆球磨珠，球磨处理24～36h，球磨后过325～500目筛，得陶瓷粘结剂粉末；
（2）依次称取300～500g冰晶石，80～100g氧化铝，30～40g碳纤维，倒入球磨机中，按球料质量比为10：1～20：1加入氧化锆球磨珠，球磨处理3～5h，再将球磨机中物料转入烘箱中，于温度为105～110℃条件下干燥至恒重，得干燥物，再将所得干燥物于压力为15～20MPa，温度为120～160℃条件下，热压成厚度为2～4mm薄片，得中间层材料；
（3）在带搅拌器的三口烧瓶中依次加入200～300g碳化硅颗粒，15～30mL质量分数为3～5%羧甲基纤维素钠溶液，以300～500r/min转速搅拌混合45～60min，在搅拌状态下，以2～4g/min速率将20～35g陶瓷粘结剂粉末添加至三口烧瓶中，待添加结束，再加入40～50g活性炭，继续搅拌混合2～4h，再将三口烧瓶中物料于压力为25～30MPa，温度为80～100℃条件下热压成厚度为8～12mm薄片，再于温度为1250～1300℃条件下，保温烧结2～4h，得支撑体材料；
（4）依次称取200～300g碳化硅粉末，40～50g陶瓷粘结剂粉末，倒入盛有400～500mL质量分数为2～4%羧甲基纤维素钠溶液的烧杯中，用玻璃棒搅拌混合30～40min，得过滤膜浆料；
（5）将中间层材料平铺于支撑体材料表面，再将所得过滤膜浆料在中间层材料表面流延成膜，控制膜厚度为280～300μm，得三层复合湿料，再将所得三层复合湿料置于烘箱中，于温度为105～110℃条件下干燥2～4h，得干燥产物；
（6）将所得干燥产物转入烧结炉，以4～6mL/min速率向炉内通入氮气，在氮气保护状态下，将干燥产物的中间层材料两端与石墨电极接通，进行保温烧结电解，待烧结电解结束，在氮气保护状态下自然冷却至室温，得烧结料；
（7）将上述所得烧结料转入盛有1～2L质量分数为2～4%醋酸溶液的烧杯中，浸泡30～45min，再用去离子水洗涤烧结料，直至洗涤液呈中性，再将洗涤后的烧结料转入烘箱中，于温度为105～110℃条件下干燥至恒重，出料，即得碳化硅多孔陶瓷过滤膜材料。
步骤（2）所述的球磨处理过程中，还可以添加冰晶石质量0.8～1.2倍的无水乙醇。
步骤（3）所述的碳化硅颗粒粒径为200～300μm。
步骤（4）所述的碳化硅粉末粒径为20～40μm。
步骤（6）所述的保温烧结电解条件为：调节石墨电极两端电压至4～6V，电流至200～300kA，再以10～20℃/min速率程序升温至980～1000℃，保温烧结电解60～90min。
本发明与其他方法相比，有益技术效果是：
（1）本发明将粒径较小的碳化硅粉末与自制陶瓷粘结剂粉末分散于羧甲基纤维素钠溶液中，制得过滤膜浆料，再将过滤膜浆料流延于以冰晶石、氧化铝及碳纤维压制成的中间层材料表面，形成薄膜，避免粒径较小的碳化硅颗粒填充进入孔隙较大的支撑体材料中，降低最终成型过滤膜材料的过滤压降程度，保证整个过滤体有足够的过滤除尘效率和精度，在对燃气轮机气体过滤时，对含尘气体的分离效率可达99.6～99.9%；
（2）本发明通过在氮气保护状态下，进行烧结电解，使中间层材料中冰晶石和氧化铝熔融电解，产生氧气，形成多孔结构的中间层，在冷却固化过程中，中间层重新固化，将上层过滤膜及下层支撑体牢固连接，在使用过程中，可有效避免过滤膜与支撑体脱离，使陶瓷过滤膜使用寿命有效延长，最终经醋酸溶液浸泡，溶解除去部分中间层电解产生的铝，丰富其空隙结构，进一步降低所得过滤膜在使用过程中的压降。
具体实施方式
依次称取100～120g高岭土，200～220g石英石，600～650g钾长石，倒入球磨机中，按球料质量比为10：1～20：1加入氧化锆球磨珠，球磨处理24～36h，球磨后过325～500目筛，得陶瓷粘结剂粉末；依次称取300～500g冰晶石，80～100g氧化铝，30～40g碳纤维，240～600g无水乙醇，倒入球磨机中，按球料质量比为10：1～20：1加入氧化锆球磨珠，球磨处理3～5h，再将球磨机中物料转入烘箱中，于温度为105～110℃条件下干燥至恒重，得干燥物，再将所得干燥物于压力为15～20MPa，温度为120～160℃条件下，热压成厚度为2～4mm薄片，得中间层材料；在带搅拌器的三口烧瓶中依次加入200～300g粒径为200～300μm的碳化硅颗粒，15～30mL质量分数为3～5%羧甲基纤维素钠溶液，以300～500r/min转速搅拌混合45～60min，在搅拌状态下，以2～4g/min速率将20～35g陶瓷粘结剂粉末添加至三口烧瓶中，待添加结束，再加入40～50g活性炭，继续搅拌混合2～4h，再将三口烧瓶中物料于压力为25～30MPa，温度为80～100℃条件下热压成厚度为8～12mm薄片，再于温度为1250～1300℃条件下，保温烧结2～4h，得支撑体材料；依次称取200～300g粒径为20～40μm的碳化硅粉末，40～50g陶瓷粘结剂粉末，倒入盛有400～500mL质量分数为2～4%羧甲基纤维素钠溶液的烧杯中，用玻璃棒搅拌混合30～40min，得过滤膜浆料；将中间层材料平铺于支撑体材料表面，再将所得过滤膜浆料在中间层材料表面流延成膜，控制膜厚度为280～300μm，得三层复合湿料，再将所得三层复合湿料置于烘箱中，于温度为105～110℃条件下干燥2～4h，得干燥产物；将所得干燥产物转入烧结炉，以4～6mL/min速率向炉内通入氮气，在氮气保护状态下，在干燥产物的中间层材料两端与石墨电极接通，调节石墨电极两端电压至4～6V，电流至200～300kA，再以10～20℃/min速率程序升温至980～1000℃，保温烧结电解60～90min，待烧结电解结束，在氮气保护状态下自然冷却至室温，得烧结料；将所得烧结料转入盛有1～2L质量分数为2～4%醋酸溶液的烧杯中，浸泡30～45min，再用去离子水洗涤烧结料，直至洗涤液呈中性，再将洗涤后的烧结料转入烘箱中，于温度为105～110℃条件下干燥至恒重，出料，即得碳化硅多孔陶瓷过滤膜材料。
实例1
依次称取100g高岭土，200g石英石，600g钾长石，倒入球磨机中，按球料质量比为10：1加入氧化锆球磨珠，球磨处理24h，球磨后过325目筛，得陶瓷粘结剂粉末；依次称取300g冰晶石，80g氧化铝，30g碳纤维，倒入球磨机中，按球料质量比为10：1加入氧化锆球磨珠，球磨处理3h，再将球磨机中物料转入烘箱中，于温度为105℃条件下干燥至恒重，得干燥物，再将所得干燥物于压力为15MPa，温度为120℃条件下，热压成厚度为2mm薄片，得中间层材料；在带搅拌器的三口烧瓶中依次加入200g粒径为200μm的碳化硅颗粒，15mL质量分数为3%羧甲基纤维素钠溶液，以300r/min转速搅拌混合45min，在搅拌状态下，以2g/min速率将20g陶瓷粘结剂粉末添加至三口烧瓶中，待添加结束，再加入40g活性炭，继续搅拌混合2h，再将三口烧瓶中物料于压力为25MPa，温度为80℃条件下热压成厚度为8mm薄片，再于温度为1250℃条件下，保温烧结2h，得支撑体材料；依次称取200g粒径为20μm的碳化硅粉末，40g陶瓷粘结剂粉末，倒入盛有400mL质量分数为2%羧甲基纤维素钠溶液的烧杯中，用玻璃棒搅拌混合30min，得过滤膜浆料；将中间层材料平铺于支撑体材料表面，再将所得过滤膜浆料在中间层材料表面流延成膜，控制膜厚度为280μm，得三层复合湿料，再将所得三层复合湿料置于烘箱中，于温度为105℃条件下干燥2h，得干燥产物；将所得干燥产物转入烧结炉，以4mL/min速率向炉内通入氮气，在氮气保护状态下，在干燥产物的中间层材料两端与石墨电极接通，调节石墨电极两端电压至4V，电流至200kA，再以10℃/min速率程序升温至980℃，保温烧结电解60min，待烧结电解结束，在氮气保护状态下自然冷却至室温，得烧结料；将所得烧结料转入盛有1L质量分数为2%醋酸溶液的烧杯中，浸泡30min，再用去离子水洗涤烧结料，直至洗涤液呈中性，再将洗涤后的烧结料转入烘箱中，于温度为105℃条件下干燥至恒重，出料，即得碳化硅多孔陶瓷过滤膜材料。
将本发明所得碳化硅多孔陶瓷过滤膜材料安装于高温陶瓷过滤器中，并将陶瓷过滤器应用于洁净煤燃烧发电过程中，于工作温度为600℃，工作压力为0.6MPa条件下，对进入燃气轮机的气体进行过滤，经检测，过滤后，进入燃气轮机的气体含尘浓度由75mg/Nm3降低至0.3mg/Nm3，分离效率达99.6%，且在使用过程中，未发现过滤膜与支撑体脱离现象，使用寿命较常规陶瓷过滤膜延长2个月。
实例2
依次称取120g高岭土，220g石英石，650g钾长石，倒入球磨机中，按球料质量比为20：1加入氧化锆球磨珠，球磨处理36h，球磨后过500目筛，得陶瓷粘结剂粉末；依次称取500g冰晶石，100g氧化铝，40g碳纤维，600g无水乙醇，倒入球磨机中，按球料质量比为20：1加入氧化锆球磨珠，球磨处理5h，再将球磨机中物料转入烘箱中，于温度为110℃条件下干燥至恒重，得干燥物，再将所得干燥物于压力为20MPa，温度为160℃条件下，热压成厚度为4mm薄片，得中间层材料；在带搅拌器的三口烧瓶中依次加入300g粒径为300μm的碳化硅颗粒，30mL质量分数为5%羧甲基纤维素钠溶液，以500r/min转速搅拌混合60min，在搅拌状态下，以4g/min速率将35g陶瓷粘结剂粉末添加至三口烧瓶中，待添加结束，再加入50g活性炭，继续搅拌混合4h，再将三口烧瓶中物料于压力为30MPa，温度为100℃条件下热压成厚度为12mm薄片，再于温度为1300℃条件下，保温烧结4h，得支撑体材料；依次称取300g粒径为40μm的碳化硅粉末，50g陶瓷粘结剂粉末，倒入盛有500mL质量分数为4%羧甲基纤维素钠溶液的烧杯中，用玻璃棒搅拌混合40min，得过滤膜浆料；将中间层材料平铺于支撑体材料表面，再将所得过滤膜浆料在中间层材料表面流延成膜，控制膜厚度为300μm，得三层复合湿料，再将所得三层复合湿料置于烘箱中，于温度为110℃条件下干燥4h，得干燥产物；将所得干燥产物转入烧结炉，以6mL/min速率向炉内通入氮气，在氮气保护状态下，在干燥产物的中间层材料两端与石墨电极接通，调节石墨电极两端电压至6V，电流至300kA，再以20℃/min速率程序升温至1000℃，保温烧结电解90min，待烧结电解结束，在氮气保护状态下自然冷却至室温，得烧结料；将所得烧结料转入盛有2L质量分数为4%醋酸溶液的烧杯中，浸泡45min，再用去离子水洗涤烧结料，直至洗涤液呈中性，再将洗涤后的烧结料转入烘箱中，于温度为110℃条件下干燥至恒重，出料，即得碳化硅多孔陶瓷过滤膜材料。
将本发明所得碳化硅多孔陶瓷过滤膜材料安装于高温陶瓷过滤器中，并将陶瓷过滤器应用于洁净煤燃烧发电过程中，于工作温度为900℃，工作压力为3.0MPa条件下，对进入燃气轮机的气体进行过滤，经检测，过滤后，进入燃气轮机的气体含尘浓度由500mg/Nm3降低至0.3mg/Nm3，分离效率达99.9%，且在使用过程中，未发现过滤膜与支撑体脱离现象，使用寿命较常规陶瓷过滤膜延长3个月。
实例3
依次称取110g高岭土，210g石英石，625g钾长石，倒入球磨机中，按球料质量比为15：1加入氧化锆球磨珠，球磨处理30h，球磨后过412目筛，得陶瓷粘结剂粉末；依次称取400g冰晶石，90g氧化铝，35g碳纤维，倒入球磨机中，按球料质量比为15：1加入氧化锆球磨珠，球磨处理4h，再将球磨机中物料转入烘箱中，于温度为108℃条件下干燥至恒重，得干燥物，再将所得干燥物于压力为18MPa，温度为140℃条件下，热压成厚度为3mm薄片，得中间层材料；在带搅拌器的三口烧瓶中依次加入250g粒径为250μm的碳化硅颗粒，22mL质量分数为4%羧甲基纤维素钠溶液，以400r/min转速搅拌混合52min，在搅拌状态下，以3g/min速率将27g陶瓷粘结剂粉末添加至三口烧瓶中，待添加结束，再加入45g活性炭，继续搅拌混合3h，再将三口烧瓶中物料于压力为28MPa，温度为90℃条件下热压成厚度为10mm薄片，再于温度为1275℃条件下，保温烧结3h，得支撑体材料；依次称取250g粒径为30μm的碳化硅粉末，45g陶瓷粘结剂粉末，倒入盛有450mL质量分数为3%羧甲基纤维素钠溶液的烧杯中，用玻璃棒搅拌混合35min，得过滤膜浆料；将中间层材料平铺于支撑体材料表面，再将所得过滤膜浆料在中间层材料表面流延成膜，控制膜厚度为290μm，得三层复合湿料，再将所得三层复合湿料置于烘箱中，于温度为108℃条件下干燥3h，得干燥产物；将所得干燥产物转入烧结炉，以5mL/min速率向炉内通入氮气，在氮气保护状态下，在干燥产物的中间层材料两端与石墨电极接通，调节石墨电极两端电压至5V，电流至250kA，再以15℃/min速率程序升温至990℃，保温烧结电解75min，待烧结电解结束，在氮气保护状态下自然冷却至室温，得烧结料；将所得烧结料转入盛有1L质量分数为3%醋酸溶液的烧杯中，浸泡38min，再用去离子水洗涤烧结料，直至洗涤液呈中性，再将洗涤后的烧结料转入烘箱中，于温度为108℃条件下干燥至恒重，出料，即得碳化硅多孔陶瓷过滤膜材料。
将本发明所得碳化硅多孔陶瓷过滤膜材料安装于高温陶瓷过滤器中，并将陶瓷过滤器应用于洁净煤燃烧发电过程中，于工作温度为750℃，工作压力为1.8MPa条件下，对进入燃气轮机的气体进行过滤，经检测，过滤后，进入燃气轮机的气体含尘浓度由288mg/Nm3降低至0.4mg/Nm3，分离效率达99.8%，且在使用过程中，未发现过滤膜与支撑体脱离现象，使用寿命较常规陶瓷过滤膜延长3个月。
Claims (5)
1.一种碳化硅多孔陶瓷过滤膜材料的制备方法，其特征在于具体制备步骤为：
（1）依次称取100～120g高岭土，200～220g石英石，600～650g钾长石，倒入球磨机中，按球料质量比为10：1～20：1加入氧化锆球磨珠，球磨处理24～36h，球磨后过325～500目筛，得陶瓷粘结剂粉末；
（2）依次称取300～500g冰晶石，80～100g氧化铝，30～40g碳纤维，倒入球磨机中，按球料质量比为10：1～20：1加入氧化锆球磨珠，球磨处理3～5h，再将球磨机中物料转入烘箱中，于温度为105～110℃条件下干燥至恒重，得干燥物，再将所得干燥物于压力为15～20MPa，温度为120～160℃条件下，热压成厚度为2～4mm薄片，得中间层材料；
（3）在带搅拌器的三口烧瓶中依次加入200～300g碳化硅颗粒，15～30mL质量分数为3～5%羧甲基纤维素钠溶液，以300～500r/min转速搅拌混合45～60min，在搅拌状态下，以2～4g/min速率将20～35g陶瓷粘结剂粉末添加至三口烧瓶中，待添加结束，再加入40～50g活性炭，继续搅拌混合2～4h，再将三口烧瓶中物料于压力为25～30MPa，温度为80～100℃条件下热压成厚度为8～12mm薄片，再于温度为1250～1300℃条件下，保温烧结2～4h，得支撑体材料；
（4）依次称取200～300g碳化硅粉末，40～50g陶瓷粘结剂粉末，倒入盛有400～500mL质量分数为2～4%羧甲基纤维素钠溶液的烧杯中，用玻璃棒搅拌混合30～40min，得过滤膜浆料；
（5）将中间层材料平铺于支撑体材料表面，再将所得过滤膜浆料在中间层材料表面流延成膜，控制膜厚度为280～300μm，得三层复合湿料，再将所得三层复合湿料置于烘箱中，于温度为105～110℃条件下干燥2～4h，得干燥产物；
（6）将所得干燥产物转入烧结炉，以4～6mL/min速率向炉内通入氮气，在氮气保护状态下，将干燥产物的中间层材料两端与石墨电极接通，进行保温烧结电解，待烧结电解结束，在氮气保护状态下自然冷却至室温，得烧结料；
（7）将上述所得烧结料转入盛有1～2L质量分数为2～4%醋酸溶液的烧杯中，浸泡30～45min，再用去离子水洗涤烧结料，直至洗涤液呈中性，再将洗涤后的烧结料转入烘箱中，于温度为105～110℃条件下干燥至恒重，出料，即得碳化硅多孔陶瓷过滤膜材料。
2.根据权利要求1所述的一种碳化硅多孔陶瓷过滤膜材料的制备方法，其特征在于：步骤（2）所述的球磨处理过程中，还可以添加冰晶石质量0.8～1.2倍的无水乙醇。
3.根据权利要求1所述的一种碳化硅多孔陶瓷过滤膜材料的制备方法，其特征在于：步骤（3）所述的碳化硅颗粒粒径为200～300μm。
4.根据权利要求1所述的一种碳化硅多孔陶瓷过滤膜材料的制备方法，其特征在于：步骤（4）所述的碳化硅粉末粒径为20～40μm。
5.根据权利要求1所述的一种碳化硅多孔陶瓷过滤膜材料的制备方法，其特征在于：步骤（6）所述的保温烧结电解条件为：调节石墨电极两端电压至4～6V，电流至200～300kA，再以10～20℃/min速率程序升温至980～1000℃，保温烧结电解60～90min。
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