CN115385714A - 一种适用于海绵城市的碳化硅陶瓷膜及其制备方法 - Google Patents

一种适用于海绵城市的碳化硅陶瓷膜及其制备方法 Download PDF

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CN115385714A
CN115385714A CN202211030981.5A CN202211030981A CN115385714A CN 115385714 A CN115385714 A CN 115385714A CN 202211030981 A CN202211030981 A CN 202211030981A CN 115385714 A CN115385714 A CN 115385714A
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silicon carbide
water
ceramic membrane
separation layer
support body
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CN115385714B (zh
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刘井雄
何龙
罗德平
曾情
唐庆凤
刘奇
贺佳
王春泉
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Jiangxi Huanyu Industrial Ceramics Technology Research Co ltd
Jiangxi Pingxiang Longfa Enterprise Co ltd
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Abstract

本发明公开了一种适用于海绵城市的碳化硅陶瓷膜，它按下述方法制备而成：先将碳化硅粉体和烧结助剂与水制备成浆料，再通过喷雾干燥的方法制备出碳化硅球形粉体，碳化硅支撑体的挤出成型：将喷雾干燥获得的碳化硅球形粉体与聚氧化乙烯混合，然后将混合料经陈腐后挤压成型，得到生坯碳化硅支撑体，烧结得到碳化硅支撑体，用碳化硅细粉、分散剂和水混合制成分离层浆料，再向分离层浆料中加入表面改性剂，混合均匀制成涂覆料，高温烧结制备出适用于海绵城市的碳化硅陶瓷膜，本发明可有效地解决城市黑臭水体及污水处理问题，加强水治理体系建设，防止和消除V类黑臭水体的持续产生，实现内涝防控和水土资源保持，为建设综合性海绵城市奠定坚实基础。

Description

一种适用于海绵城市的碳化硅陶瓷膜及其制备方法
技术领域
本发明涉及陶瓷制品，具体涉及一种适用于海绵城市的碳化硅陶瓷膜。
背景技术
目前很多的老工业城市都存在老城区建设高度密集、空间布局不合理、城市基础设施历史欠账多等问题。由此产生的城市黑臭水体是会对城市的人居环境和城市形象造成较大的负面影响。
海绵城市理念的提出及建设为解决城市黑臭水体及污水处理问题提供了新理念及方向。通过海绵城巿建设,综合采取“渗、滞、蓄、净、用、排”等措施,最大限度地减少城市开发建设对生态环境的影响。海绵城市建设的目标就是要紧紧把握积存、渗透及净化的自然性，并实现对雨水资源的收集和加强水环境污染治理，以保证水资源的平衡发展。在城市黑臭水体整治技术应用过程中，要建立统筹水资源，加强水治理体系建设，防止和消除V 类黑臭水体的持续产生，实现内涝防控和水土资源保持，为建设综合性海绵城市奠定坚实基础。
因此在建设海绵城市开展黑臭水体治理时，需要结合实际情况，在工程中应用的海绵设施主要包括以下几种：第一种设施是—截污式水口：即通过对现状水口加装截污设施改造成截污式水口，来拦截进入水管道的垃圾、颗粒污染物；第二种是雨水管断接：将建筑屋面雨水引入到周边绿地设置的分散式雨水控制利用设施内进行下渗、净化；第三种是下沉式绿地/雨水花园：利用现状绿地空间，建设具有截留净化能力的生物滞留设施，消纳、滞留雨水径流。
针对上述三种主要情况，采取什么新型材料制成截污式水口、分散式雨水控制利用设施、下沉式绿地/雨水花园来解决城市黑臭水体及污水处理问题，实现对雨水资源的收集和加强水环境污染治理，以保证水资源的平衡发展，这是目前环保技术领域中急需要解决的技术问题。
发明内容
针对上述现有技术中所面临的问题，本发明提供了一种适用于海绵城市建设的通过改性制成的新型碳化硅陶瓷膜材料。
本发明所述SiC具有高机械强度、耐高温、高热导率、较低的热膨胀系数及优异的化学惰性，其在膜领域应用的最大优势在于其耐高温和耐酸碱腐蚀。纯SiC在1500℃的高温下强度不下降反而升高20~30%，可在1600℃高温空气条件下长时间使用。SiC几乎能在至今所知的所有腐蚀性水溶液中稳定存在，仅被215℃的磷酸和100℃以上K3Fe(CN)6的碱溶液轻微腐蚀。SiC中存在缺陷时才被熔融碱选择性腐蚀，多孔SiC在沸腾的5mol/L硝酸中腐蚀后，与腐蚀前相比几乎没有任何差异。SiC将是高浓度酸（碱）热液、高温气体分离、高温烟气过滤及高温熔体过滤等苛刻应用环境下膜材料的必然选择。
非对称梯度结构碳化硅陶瓷膜具有高机械强度、耐高温、高热导率、较低的热膨胀系数及优异的化学惰性，其几乎能在至今所知的所有腐蚀性水溶液中稳定存在。可以解决高浓度酸（碱）热液、高温气体分离、高温烟气过滤及高温熔体过滤等苛刻应用环境面临的浓缩分离和高温除尘等技术难题，为化工、冶金、电力、石油等行业的废水处理回用和原油加工、石化产品生产等行业的有机溶剂回用处理，市政供水水质净化及市政污水回用、医药、植物提取、氯碱、乳品、糖醇、高温烟气处理、柴油车尾气处理、PM2.5捕获收集等领域提供重要的材料支撑，也为高浓粘物料的分离澄清提供新技术思路，解决其效率低、易堵塞、高耗能等问题。同时，碳化硅具有良好的亲水性能，对生活、工业生产各个领域具备巨大的经济价值，同时在海绵城市建设中解决城市黑臭水体方面具备广泛的应用。
一种适用于海绵城市的碳化硅陶瓷膜，它按下述方法步骤制备而成：
（1）碳化硅原料造粒：先将碳化硅粉体和烧结助剂与水按比例制备成浆料，再通过喷雾干燥的方法制备出碳化硅球形粉体，所述烧结助剂为碳化硼、氧化铝、氧化钇、氧化硅一种或者多种，
（2）碳化硅支撑体的挤出成型：将喷雾干燥获得的碳化硅球形粉体与聚氧化乙烯、甲基纤维素、乙基纤维素、乙氧基化合物、三油酸甘油酯、聚丙烯酸甲酯、聚甲基丙烯酸中的一种或者多种混合均匀，然后将混合料经陈腐后挤出成型，得到生坯碳化硅支撑体，
（3）支撑体的干燥：将生坯碳化硅支撑体置于微波干燥炉中干燥，
（4）高温烧结：将干燥后的生坯碳化硅支撑体进行烧结，得到碳化硅支撑体，
（5）分离层的改性和一次烧成：先用碳化硅细粉、占碳化硅细粉重量0.5-10%的分散剂和适量的水混合制成分离层浆料，再向分离层浆料中加入用二氧化硅、三氧化二铁、二氧化钛、二氧化锡、五氧化二钒中的一种或者多种制成的表面改性剂，混合均匀制成涂覆料，再将涂覆料喷涂在碳化硅支撑体表面上形成分离层，微波干燥后，经一次高温烧结形成核壳包覆结构，制备出适用于海绵城市建设的碳化硅陶瓷膜。
所述烧结助剂在烧结过程中通过取代形成空位、产生液相等方式降低烧结的物质迁移活化能，促进烧结的发生，降低烧成温度，减小生产成本，增强材料的强度。
本发明的技术效果：本发明采用高机械强度、耐高温、高热导率、较低的热膨胀系数及优异的化学惰性的微细碳化硅颗粒与分散剂和水混合形成胶料并喷涂在支撑体表面上形成核壳包覆层，并使核壳包覆层改性形成具有连通的微孔和大通量的分离层。它与传统非对称陶瓷膜相比，减少了中间层，能有效减少过滤阻力，增大陶瓷膜的通量，且实现了表面包覆改性和分离层的一次烧成，将传统制备方法的三次（支撑体烧结、包覆烧结和分离层烧结）减少为两次烧结（支撑体烧结、包覆和分离一次烧结），能降低能耗，降低生产成本。经包覆改性后的碳化硅陶瓷膜具有优异的亲水性能，能有效降低陶瓷膜的过滤阻力，提高其通量和抗污能力，本发明应用于海绵城市建设中可有效地解决城市黑臭水体及污水处理问题，建立统筹水资源，加强水治理体系建设，防止和消除V 类黑臭水体的持续产生，把握积存、渗透及净化的自然性，实现内涝防控和水土资源保持，为建设综合性海绵城市奠定坚实基础，实现对雨水资源的收集和加强水环境污染治理，以保证水资源的平衡发展。
附图说明
图1是碳化硅陶瓷膜核壳包覆结构示意图，
图2 是管式碳化硅陶瓷膜管件的立体结构示意图，
图3是管式碳化硅陶瓷膜连通孔显微结构图，
图4平板碳化硅陶瓷膜板的立体结构示意图，
图5是平板碳化硅陶瓷膜连通孔显微结构图。
在图中， 1、分离层 2、碳化硅球形粉体。
具体实施方式
实施例1，如图1、图2和图3所示，一种适用于海绵城市的管式碳化硅陶瓷膜，所述管式碳化硅陶瓷膜内部为连通孔结构，平均孔径为150 nm，外形为Φ60mm×1200mm，纯水通量为3.2 m3/(m2·h)，经原料造粒-挤出成型-微波干燥-烧结-覆膜制备而成。具体按下述方法步骤制备而成：
（1）用碳化硅原料进行造粒：用65wt%的碳化硅粗粉（150-300目）为骨架，用5wt%的烧结助剂和30wt%的碳化硅细粉（6000目）及适量的水与碳化硅粗粉混合制成浆料，使烧结助剂填充在粗粉与粗粉所形成的空隙内，再将浆料通过喷雾干燥的方法制备出碳化硅球形粉体2（或碳化硅颗粒2），所述烧结助剂用50wt%的氧化铝、10wt%氧化钇和40wt%氧化硅混合制成，
（2）碳化硅支撑体的挤出成型：将喷雾干燥获得的碳化硅球形粉体与占碳化硅球形粉体重量5%的聚氧化乙烯和甲基纤维素（重量各占50%）两种物质均匀混合，然后将混合料经陈腐20-24小时，再用管式模具体挤出成型，得到管式生坯碳化硅支撑体，
（3）支撑体的干燥：将管式生坯碳化硅支撑体置于微波干燥炉中干燥至水分小于1%，
（4）高温烧结：将干燥后的管式生坯碳化硅支撑体在1700-1800℃下保温烧结10-15小时，冷却得到管式碳化硅支撑体，
（5）分离层的改性和一次烧成：先用碳化硅细粉、占碳化硅细粉重量0.5-10%（优选1.5%）的分散剂和适量的水混合制成分离层浆料，再在分离层浆料中加入由重量比为2∶3∶1的二氧化硅、三氧化二铁、二氧化钛混合制成的表面改性剂（表面改性剂加入量为分离层浆料重量的3%），经混合均匀制成涂覆料，再将涂覆料喷涂在支撑体表面上（管两端孔用封堵剂封闭）形成分离层（即包覆改变性层），微波干燥后，经一次高温（1500-1600℃）保温2-4小时烧结形成核壳包覆结构（即包覆改性层），制备出适用于海绵城市建设使用的管式碳化硅陶瓷膜。适量的水是指能使分离浆料呈稠状时的水量，所述分散剂为六偏磷酸钠、焦磷酸钠、氨水、乙酸乙脂或聚乙烯酸钠盐等一种或多种。所述分离层陶瓷膜孔径范围为100nm~1μm，分离层（即包覆改性层）厚度为300nm~30μm。
实施例2，如图1、图4和图5所示，一种适用于海绵城市的平板式碳化硅陶瓷膜，所述管式碳化硅陶瓷膜内部为连通孔结构，平均孔径为106 nm，外形为500mm×500mm×8.5mm，纯水通量为2.9m3/(m2·h)，经原料造粒-挤出成型-微波干燥-烧结-覆膜制备而成。具体按下述方法步骤制备而成：
（1）用碳化硅原料进行造粒：用55wt%的碳化硅粗粉（150-300目）为骨架，用5wt%的烧结助剂和40wt%的碳化硅细粉（6000目）及适量的水与碳化硅粗粉混合制成浆料，使烧结助剂填充在粗粉与粗粉所形成的空隙内，再将浆料通过喷雾干燥的方法制备出碳化硅球形粉体2（或碳化硅颗粒2），所述烧结助剂用60wt%的氧化铝和40wt%碳化硼混合制成，
（2）碳化硅支撑体的挤出成型：将喷雾干燥获得的碳化硅球形粉体与占碳化硅球形粉体重量8%的甲基纤维素、乙基纤维素、乙氧基化合物、三油酸甘油酯（四种重量依次为40%、30%、15%、15%）四种物质均匀混合，然后将混合料经陈腐20-24小时，再用平板式模具体挤出成型，得到平板式生坯碳化硅支撑体，
（3）支撑体的干燥：将平板式生坯碳化硅支撑体置于微波干燥炉中干燥至水分小于1%，
（4）高温烧结：将干燥后的平板式生坯碳化硅支撑体在1900-2000℃下保温烧结10-15小时，冷却得到平板式碳化硅支撑体，
（5）分离层的改性和一次烧成：先用碳化硅细粉、占碳化硅细粉重量0.5-10%（优选5%）的分散剂和适量的水混合制成分离层浆料，再在分离层浆料中加入由重量比为2∶3∶1∶1的二氧化硅、三氧化二铁、二氧化钛、五氧化二钒四种混合制成的表面改性剂（表面改性剂加入量为分离层浆料重量的5%），并混合均匀制成涂覆料，再将涂覆料喷涂在支撑体表面上（四侧的出水孔用封堵剂封闭）形成分离层1，微波干燥后，经一次高温（1500-1600℃）保温2-4小进烧结形成核壳包覆结构（即包覆改性层），制备出适用于海绵城市的碳化硅陶瓷膜。适量的水量是指分离浆料呈稠状时的水量，所述分散剂为六偏磷酸钠、焦磷酸钠、氨水、乙酸乙脂或聚乙烯酸钠盐等中一种或多种。所述分离层陶瓷膜孔径范围为100nm~1μm，分离层（即包覆改性层）厚度为300nm~30μm。

Claims (3)

1.一种适用于海绵城市的碳化硅陶瓷膜，其特征在于：它按下述方法步骤制备而成：
（1）碳化硅原料造粒：先将碳化硅粉体和烧结助剂与水按比例的制备成浆料，再通过喷雾干燥的方法制备出碳化硅球形粉体（2），所述烧结助剂为碳化硼、氧化铝、氧化钇、氧化硅一种或者多种，
（2）碳化硅支撑体的挤出成型：将喷雾干燥获得的碳化硅球形粉体与聚氧化乙烯、甲基纤维素、乙基纤维素、乙氧基化合物、三油酸甘油酯、聚丙烯酸甲酯、聚甲基丙烯酸中的一种或者多种均匀混合，然后将混合料经陈腐后挤压成型，得到生坯碳化硅支撑体，
（3）支撑体的干燥：将生坯碳化硅支撑体置于微波干燥炉中干燥，
（4）高温烧结：将干燥后的生坯碳化硅支撑体进行烧结，得到碳化硅支撑体，
（5）分离层的改性和一次烧成：先用碳化硅细粉、占碳化硅细粉重量0.5-10%的分散剂和适量的水混合制成分离层浆料，再向分离层浆料中加入由二氧化硅、三氧化二铁、二氧化钛、二氧化锡、五氧化二钒中的一种或者多种混合制成的表面改性剂，混合均匀制成涂覆料，再将涂覆料喷涂在碳化硅支撑体表面上形成分离层（1），微波干燥后，经一次高温烧结形成核壳包覆结构，制备出适用于海绵城市的碳化硅陶瓷膜。
2.根据权利要求1所述的一种适用于海绵城市的碳化硅陶瓷膜，其特征在于：所述分离层（1）陶瓷膜孔径为100nm~1μm，分离层厚度为300nm~30μm。
3.根据权利要求1所述的一种适用于海绵城市的碳化硅陶瓷膜，其特征在于：所述分散剂为六偏磷酸钠、焦磷酸钠、氨水、四甲基氢氧化铵、乙酸乙脂或聚乙烯酸钠盐中一种或多种。
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