CN112090170B - 一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法 - Google Patents
一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法 Download PDFInfo
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Abstract
本发明属于属于氧化锌材料技术领域，尤其是一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法，利用聚腙和氧化锌进行复合制备氧化锌滤芯材料，电子与空穴简单复合的概率降低，光催化活性增大，在高能高臭氧UV紫外线光束照射恶臭气体和氧化锌滤芯光催化，催化裂解恶臭气体如：硫化氢、甲硫氢、甲硫醇、二甲二硫、二硫化碳、硫化物H2S、VOC类，使有机或无机高分子恶臭化合物分子链，在高能紫外线光束照射下，降解转变成低分子化合物。
Description
技术领域
本发明属于氧化锌材料技术领域，尤其是一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法。
背景技术
一切刺激嗅觉器官引起人们不愉快及损坏生活环境的气体物质为恶臭。为了保护和提高各类处理现场及周围环境卫生质量，减少对空气造成的二次污染，对恶臭进行有效的控制是十分必要的。从恶臭处理效果、工程投资、运行成本、自控程度、占地大小和有无二次污染等方面，紫外光冷燃烧除臭具有较好的应用价值，运用高能UV紫外线光束及臭氧对恶臭气体进行协同分解氧化反应,使恶臭气体物质其降解化成低分子化合物、水和二氧化碳，中国专利CN208604028U公开了底端设置有紫外光冷燃烧除臭设备的用于畜禽养殖废弃物资源化处理设备，中国专利CN101612522公开了一种利用臭氧、紫外线处理恶臭气体的装置和方法，由过滤网、臭氧发生器、强力混合器、紫外光化氧化反应器、除臭氧尾气装置和风机组成，在紫外灯和触媒、氧化用下，恶臭分子被转化为二氧化碳和水，来实现臭气的达标排放，现有的滤芯材料有活性炭、沸石，而活性炭吸附能力强的有机废气置换吸附能力弱的有机废气，从而形成部分污染因子在局部的浓度高于进气浓度的现象，同比单组分有机废气，活性炭吸附多组分有机气体的效率会下降，沸石孔道较窄，不利于大分子吸附，三甲胺、硫化氢、甲硫氢、甲硫醇、二甲二硫、二硫化碳和苯乙烯，硫化物H2S、VOC类，苯、甲苯、二甲苯的分子链结构，使有机或无机高分子恶臭化合物分子链，在高能紫外线光束照射下，降解转变成低分子化合物，但目前的紫外光冷燃烧除臭滤芯工能单一，且除臭效率并不高，造成了滤芯造价成本高，且除臭设备的大小尺寸收到限制，本领域技术人员亟待开发出一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法。
发明内容
针对上述问题，本发明旨在提供一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法。
一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法，包括以下步骤：
（1）聚腙的制备：按重量份数计，将45~53份的去离子水加入带有回流冷凝管、温度计、滴液漏斗的反应釜中，再加入亚硫酸氢钠0.01~0.02份，匀速滴加丙烯酸类单体23~26份及质量分数1~2%的引发剂水溶液10~12份40~50min滴完，搅拌反应1~2h，反应温度50~60℃，反应时间1~2h后，加入水合肼25~33份继续搅拌搅拌0.5~1h后，加入苯甲醛35~37份，继续搅拌0.5~1h，搅拌均匀后，65~70℃干燥至恒重，得聚腙粉末；
（2）按重量份数计，称取21~23份乙酸锌，先加57~62份冰醋酸搅拌溶解，得冰醋酸溶液，将聚腙粉末、壳聚糖4~6份、聚赖氨酸2~4份、聚乙烯亚胺1~2份加入上述冰醋酸溶液中，搅拌过夜而形成质量分数为26~31%的聚腙溶液，加入催化剂，并在置于80~95℃的恒温水浴锅中加热，陈化10~20min，白色沉淀生成，沉淀用去离子水冲洗，搅拌得凝胶颗粒悬浮液；（3）将步骤（2）得到悬浮液进口温度280~310℃、出口温度90~110℃，负压10~20Pa，送料泵转速600~800r/min，雾化器转速3000r/min，进行喷雾造粒，即得。
进一步的，所述丙烯酸类单体为丙烯酸、甲基丙烯酸中的其中一种。
进一步的，所述催化剂为乌洛托品、三乙烯二胺中的其中一种。
进一步的，所述引发剂为偶氮二异丁脒盐酸盐、过硫酸钾、过硫酸铵中的其中一种。
丙烯酸为原料制备聚合物腙的制备路线如下：
本发明的有益效果：
本发明公开的制备方法使用了聚腙，腙基团因其易于合成以及结构和功能的多样性的特点在阴/阳离子识别，金属配位作用，本发明通过自由基引发聚合，苯甲醛反应等一系列合成步骤制备含有腙基团的聚合物，该种聚合物溶于醋酸，且具有多种反应活性位点基团，溶于醋酸后，与同样溶于醋酸的醋酸锌，在碱性催化剂作用下原位生成氧化锌，同时聚合腙也在醋酸溶液条件改变后析出形成含有负载氧化锌的聚合腙，经喷雾造粒，得紫外光冷燃烧除臭氧化锌滤芯材料，制备方法简单易行，原料来源广泛。
相比现有技术本发明具有如下优点：
本发明使用氧化锌直接带隙宽禁带半导体材料进行杂化，原料廉价易得，外延生长温度低，易于掺杂，并且氧化锌可由醋酸锌制备，利用醋酸锌溶于醋酸且聚腙在醋酸中的溶解性较好的特点，使用含有聚腙的醋酸锌醋酸溶液同步掺杂氧化锌，而聚腙作为粘结骨架，起到辅助氧化锌滤芯成型的作用，同时其具有刺激反应活性，电子与空穴简单复合的概率降低，光催化活性增大，在高能高臭氧UV紫外线光束照射恶臭气体和氧化锌滤芯光催化，催化裂解恶臭气体如：氮、三甲胺、硫化氢、甲硫氢、甲硫醇、二甲二硫、二硫化碳和苯乙烯，硫化物H2S、VOC类，使有机或无机高分子恶臭化合物分子链，在高能紫外线光束照射下，降解转变成低分子化合物。
具体实施方式
下面用具体实施例说明本发明，但并不是对本发明的限制。
实施例1
（1）聚腙的制备：按重量份数计，将53份的去离子水加入带有回流冷凝管、温度计、滴液漏斗的反应釜中，再加入亚硫酸氢钠0.02份，匀速滴加丙烯酸单体26份及质量分数2%的引发剂过硫酸铵水溶液12份50min滴完，搅拌反应1h，反应温度60℃，反应时间2h后，加入水合肼33份继续搅拌搅拌1h后，加入苯甲醛35份，继续搅拌1h，搅拌均匀后，70℃干燥至恒重，得聚腙粉末；（2）按重量份数计，称取23份乙酸锌，先加62份冰醋酸搅拌溶解，得冰醋酸溶液，将聚腙粉末、壳聚糖6份、聚赖氨酸4份、聚乙烯亚胺2份加入上述冰醋酸溶液中，搅拌过夜而形成质量分数为31%的聚腙溶液，加入催化剂三乙烯二胺，并在置于95℃的恒温水浴锅中加热，陈化20min，白色沉淀生成，沉淀用去离子水冲洗，搅拌得凝胶颗粒悬浮液；（3）将步骤（2）得到悬浮液进口温度310℃、出口温度110℃，负压20Pa，送料泵转速800r/min，雾化器转速3000r/min，进行喷雾造粒，即得。
（2）聚乙烯亚胺购自江苏梦得新材料科技有限公司的MDG1500，聚赖氨酸购自伟日生物科技有限公司，壳聚糖脱乙酰度95%，分子量5万购自江苏采薇生物科技有限公司。
实施例2
（1）聚腙的制备：按重量份数计，将45份的去离子水加入带有回流冷凝管、温度计、滴液漏斗的反应釜中，再加入亚硫酸氢钠0.01份，匀速滴加甲基丙烯酸单体23份及质量分数1%的引发剂偶氮二异丁脒盐酸盐水溶液10份40min滴完，搅拌反应1h，反应温度50℃，反应时间1h后，加入水合肼25份继续搅拌搅拌0.5h后，加入苯甲醛37份，继续搅拌0.5h，搅拌均匀后，65℃干燥至恒重，得聚腙粉末；（2）按重量份数计，称取21份乙酸锌，先加57份冰醋酸搅拌溶解，得冰醋酸溶液，将聚腙粉末、聚赖氨酸4份、聚乙烯亚胺2份、壳聚糖4份加入上述冰醋酸溶液中，搅拌过夜而形成质量分数为26%的聚腙溶液，加入催化剂乌洛托品，并在置于95℃的恒温水浴锅中加热，陈化10min，白色沉淀生成，沉淀用去离子水冲洗，搅拌得凝胶颗粒悬浮液；（3）将步骤（2）得到的悬浮液进口温度280℃、出口温度90℃，负压10Pa，送料泵转速600r/min，雾化器转速3000r/min，进行喷雾造粒，即得。
聚乙烯亚胺购自江苏梦得新材料科技有限公司的MDG1500，聚赖氨酸购自伟日生物科技有限公司，壳聚糖脱乙酰度95%，分子量5万购自江苏采薇生物科技有限公司，偶氮二异丁脒盐酸盐选用苏州启航生物科技有限公司的V-50。
对比实施例1
本对比实施例1与实施例2相比，步骤（2）中省去聚腙粉末，除此外的方法步骤均相同。
对比实施例2
本对比实施例2与实施例2相比，步骤（2）中省去壳聚糖，除此外的方法步骤均相同。
对比实施例3
本对比实施例3与实施例2相比，步骤（2）中省去聚乙烯亚胺，除此外的方法步骤均相同。
对比实施例4
本对比实施例4与实施例2相比，步骤（2）中省去聚赖氨酸，除此外的方法步骤均相同。
将实施例1~2和对比例1~4的紫外光冷燃烧除臭氧化锌滤芯材料进行性能，测试结果如表1所示：
表1实施例1~2和对比例1~4的紫外光冷燃烧除臭氧化锌滤芯材料的性能测试结果
注：磨耗率的测定按HG/T2976化肥催化剂磨耗率的测定的规定进行测定；穿透硫容的测定按HG/T2513氧化锌脱硫剂硫容试验方法的规定进行测定4.4平均抗测压强度的测定按HG/T2782中规定的方法进行。
Claims (4)
1.一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法，其特征在于，包括以下步骤：
（1）聚腙的制备：按重量份数计，将45~53份的去离子水加入带有回流冷凝管、温度计、滴液漏斗的反应釜中，再加入亚硫酸氢钠0.01~0.02份，匀速滴加丙烯酸类单体23~26份及质量分数1~2%的引发剂水溶液10~12份40~50min滴完，搅拌反应1~2h，反应温度50~60℃，反应时间1~2h后，加入水合肼25~33份继续搅拌搅拌0.5~1h后，加入苯甲醛35~37份，继续搅拌0.5~1h，搅拌均匀后，65~70℃干燥至恒重，得聚腙粉末；
（2）按重量份数计，称取21~23份乙酸锌，先加57~62份冰醋酸搅拌溶解，得冰醋酸溶液，将聚腙粉末、壳聚糖4~6份、聚赖氨酸2~4份、聚乙烯亚胺1~2份加入上述冰醋酸溶液中，搅拌过夜而形成质量分数为26~31%的聚腙溶液，加入催化剂，并在置于80~95℃的恒温水浴锅中加热，陈化10~20min，白色沉淀生成，沉淀用去离子水冲洗，搅拌得凝胶颗粒悬浮液；（3）将步骤（2）得到的悬浮液进口温度280~310℃、出口温度90~110℃，负压10~20Pa，送料泵转速600~800r/min，雾化器转速3000r/min，进行喷雾造粒，即得。
2.根据权利要求1所述的一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法，其特征在于，所述丙烯酸类单体为丙烯酸、甲基丙烯酸中的其中一种。
3.根据权利要求1所述的一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法，其特征在于，所述催化剂为乌洛托品、三乙烯二胺中的其中一种。
4.根据权利要求1所述的一种紫外光冷燃烧除臭氧化锌滤芯材料的制备方法，其特征在于，所述引发剂为偶氮二异丁脒盐酸盐、过硫酸钾、过硫酸铵中的其中一种。
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