CN108559654B - 一种农业种植污水处理用滤料清洗剂的制备方法 - Google Patents
一种农业种植污水处理用滤料清洗剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种农业种植污水处理用滤料清洗剂的制备方法，涉及清洗剂领域；包括以下步骤：(1)将棉花秸秆粉、大豆淀粉和乙烯基三乙氧基硅烷混合均匀，在氮气保护气氛炉中烧结；(2)向混合物中加入改性氧化铝分子筛、活性炭、聚四氟乙烯、硅酸镁混合均匀，球磨；(3)用压力机将上述制备的混合物压制成薄块，在高温高压环境下定型，然后喷洒硫酸铜溶液；(4)向上述制备的混合物中加入月桂醇硫酸钠、脂肪醇聚氧乙烯醚和碳酸氢钠混合烧结，冷却，研磨；(5)将上述制备的混合物溶于去离子水中，滴加盐酸至PH值在5‑6之间；制备的清洗剂能够去除滤料吸附的有害物质，实现滤料重复再利用，节约资源，降低污水净化成本。
Description
技术领域：
本发明涉及清洗剂领域，具体涉及一种农业种植污水处理用滤料清洗剂的制备方法。
背景技术：
种植业是农业的主要组成部分之一，以土地为重要生产资料，利用绿色植物，通过光合作用把自然界中的二氧化碳、水和矿物质合成有机物质，同时，把太阳能转化为化学能贮藏在有机物质中。包括各种农作物、林木、果树、药用和观赏等植物的栽培。有粮食作物、经济作物、蔬菜作物、绿肥作物、饲料作物、牧草、花卉等园艺作物。
种植业中的污水主要是有生活污水、降水、种植污水等。其中废水中主要含有因浇水灌溉从植物上脱落的枝叶和自然凋谢的花瓣等，因排入河流水体中由于自身慢慢腐烂会对水体产生影响，产生大量的细菌以及含氮有机物，使水体变为浑浊甚至产生恶臭，使水体产生富营养化，甚至可能发生水华现象，有一定的危害。
目前对废水的处理方式主要有物理法、化学法和生物法，其中物理法是采用具有吸附作用的滤料对污水进行吸附过滤，达到去除有害物质的目的，滤料长期使用，使得滤料也会造成二次污染，如果直接丢弃，势必会对环境造成污染。
发明内容：
本发明所要解决的技术问题在于提供一种农业种植污水处理用滤料清洗剂的制备方法，制备的清洗剂能够去除滤料吸附的有害物质，不仅避免了对环境造成二次污染，而且能实现滤料重复再利用，节约资源，降低污水净化成本。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种农业种植污水处理用滤料清洗剂的制备方法，包括以下步骤：
(1)将棉花秸秆粉、大豆淀粉和乙烯基三乙氧基硅烷混合均匀，在400-600℃氮气保护气氛炉中烧结2-3h，降温到150-200℃时，停止通入氮气，在空气中降低到室温；
(2)向步骤(1)混合物中加入改性氧化铝分子筛、活性炭、聚四氟乙烯、硅酸镁混合均匀，放入行星式球磨机中在乙醇为球磨介质下球磨40min，球磨转速为300r/min，球磨后清洗，干燥；
(3)用压力机将步骤(2)制备的混合物压制成直径为2cm、厚度为0.3cm的薄块，将薄块于140-160℃、0.36-0.52Mpa高温高压下定型20min，然后向薄块表面喷洒8％质量浓度的硫酸铜溶液，冷却到室温，干燥、粉碎；
(4)向步骤(3)制备的混合物中加入月桂醇硫酸钠、脂肪醇聚氧乙烯醚和碳酸氢钠，在200-300℃电阻炉中烧结20min，自然冷却到室温，研磨，过200目筛；
(5)将步骤(4)制备的混合物溶于去离子水中，向溶液中滴加盐酸至PH值在5-6之间，制得所述清洗剂。
所述步骤(2)球磨过程选用碳化硅磨球，磨球直径为8mm，磨球、磨料和乙醇的质量比为1.4：1：0.5。
各原料按照以下重量份的比例组成：改性氧化铝分子筛50-70份、棉花秸秆粉80-100份、大豆淀粉25-30份、碳酸氢钠13-15份、活性炭20-30份、聚四氟乙烯5-7份、乙烯基三乙氧基硅烷2-3份、硅酸镁3-4份、月桂醇硫酸钠80-100份、脂肪醇聚氧乙烯醚50-60份、硫酸铜7-8份、盐酸适量、去离子水1000-1500份。
所述改性氧化铝分子筛的改性方法为：
(1)将氧化铝分子筛和碳纤维、焦麻纤维、聚乳酸混合均匀，在600-700℃电阻炉中保温烧结2-3h，自然冷却到室温；
(2)将步骤(1)制备的氧化铝分子筛和碳酸氢铵混合均匀，在真空炉中加热到120-125℃，保温1h，自然冷却到室温；
(3)将步骤(2)制备的氧化铝分子筛放入4-5％质量浓度的醋酸溶液中浸泡40-60min，用去离子水清洗，干燥；
(4)将步骤(3)处理后的氧化铝分子筛在真空炉中加热到600-700℃，向真空炉中循环通入氮气，保温循环30min后开始降温，同时停止通入氮气，当温度降低到300-400℃时向真空炉中循环通入二氧化碳，保温循环20min后继续降温到室温，制得改性氧化铝分子筛。
步骤(1)所述氧化铝分子筛和碳纤维、焦麻纤维、聚乳酸的质量比为500-600：17-19：7-8：11-13，步骤(2)所述氧化铝分子筛和碳酸氢铵的质量比为10：1。
本发明提供了农业种植污水处理用滤料清洗剂的制备方法，其有益效果为：
(1)制备方法采用原料逐步添加方式，首先将棉花秸秆粉、大豆淀粉和乙烯基三乙氧基硅烷在保护气氛炉中烧结，能够将原料紧密结合在一起，且不会发生高温分解，然后继续添加改性氧化铝分子筛、活性炭、聚四氟乙烯、硅酸镁，进行球磨，细化原料晶粒的同时，增加原料间的结合力，再转入高温高压环境下活化各原料，压块后喷洒硫酸铜，使硫酸铜浸润到薄块中，赋予薄块具有杀菌效果，最后放入月桂醇硫酸钠、脂肪醇聚氧乙烯醚和碳酸氢钠，使原料进一步结合的同时，在原料内部产生孔洞，使结构变的疏松，增大清洗剂与滤料接触面积，提高清洗效率。
(2)氧化铝分子筛经过改性后吸附面积会进一步增大，因而能够提高清洗剂的清洗效率。
(3)本发明清洗剂是采用分子筛、植物秸秆、淀粉、表面活性剂、造孔剂为主要原料制备而成的酸性清洗剂，分子筛能够反吸附滤料表面吸附的污水悬浮物，植物秸秆使得清洗剂能够洗去滤料中的微生物，淀粉起到增强原料结合力的作用，表面活性剂去除滤料表面的油污，酸性环境有利于去除滤料中吸附的重金属，造孔剂能够增大清洗剂的孔洞，增大清洗面积，增强清洗效果。
具体实施方式：
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例1：
一种农业种植污水处理用滤料清洗剂的制备方法，包括以下步骤：
(1)将80份棉花秸秆粉、25份大豆淀粉和2份乙烯基三乙氧基硅烷混合均匀，在400℃氮气保护气氛炉中烧结2h，降温到150℃时，停止通入氮气，在空气中降低到室温；
(2)向步骤(1)混合物中加入60份改性氧化铝分子筛、25份活性炭、6份聚四氟乙烯、3份硅酸镁混合均匀，放入行星式球磨机中在乙醇为球磨介质下球磨40min，球磨转速为300r/min，球磨后清洗，干燥；
(3)用压力机将步骤(2)制备的混合物压制成直径为2cm、厚度为0.3cm的薄块，将薄块于140℃、0.36Mpa高温高压下定型20min，然后向薄块表面喷洒7份8％质量浓度的硫酸铜溶液，冷却到室温，干燥、粉碎；
(4)向步骤(3)制备的混合物中加入90份月桂醇硫酸钠、55份脂肪醇聚氧乙烯醚和14份碳酸氢钠，在250℃电阻炉中烧结20min，自然冷却到室温，研磨，过200目筛；
(5)将步骤(4)制备的混合物溶于1000去离子水中，向溶液中滴加盐酸至PH值在5-6之间，制得所述清洗剂。
所述步骤(2)球磨过程选用碳化硅磨球，磨球直径为8mm，磨球、磨料和乙醇的质量比为1.4：1：0.5。
实施例2：
一种农业种植污水处理用滤料清洗剂的制备方法，包括以下步骤：
(1)将100份棉花秸秆粉、30份大豆淀粉和3份乙烯基三乙氧基硅烷混合均匀，在600℃氮气保护气氛炉中烧结3h，降温到200℃时，停止通入氮气，在空气中降低到室温；
(2)向步骤(1)混合物中加入70份改性氧化铝分子筛、30份活性炭、7份聚四氟乙烯、4份硅酸镁混合均匀，放入行星式球磨机中在乙醇为球磨介质下球磨40min，球磨转速为300r/min，球磨后清洗，干燥；
(3)用压力机将步骤(2)制备的混合物压制成直径为2cm、厚度为0.3cm的薄块，将薄块于150℃、0.43Mpa高温高压下定型20min，然后向薄块表面喷洒8份8％质量浓度的硫酸铜溶液，冷却到室温，干燥、粉碎；
(4)向步骤(3)制备的混合物中加入100份月桂醇硫酸钠、60份脂肪醇聚氧乙烯醚和15份碳酸氢钠，在300℃电阻炉中烧结20min，自然冷却到室温，研磨，过200目筛；
(5)将步骤(4)制备的混合物溶于1500去离子水中，向溶液中滴加盐酸至PH值在5-6之间，制得所述清洗剂。
所述步骤(2)球磨过程选用碳化硅磨球，磨球直径为8mm，磨球、磨料和乙醇的质量比为1.4：1：0.5。
所述改性氧化铝分子筛的改性方法为：
(1)将氧化铝分子筛和碳纤维、焦麻纤维、聚乳酸按照质量比为600：19：7：13混合均匀，在600℃电阻炉中保温烧结3h，自然冷却到室温；
(2)将步骤(1)制备的氧化铝分子筛和碳酸氢铵按照质量比为10：1混合均匀，在真空炉中加热到125℃，保温1h，自然冷却到室温；
(3)将步骤(2)制备的氧化铝分子筛放入4％质量浓度的醋酸溶液中浸泡60min，用去离子水清洗，干燥；
(4)将步骤(3)处理后的氧化铝分子筛在真空炉中加热到600℃，向真空炉中循环通入氮气，保温循环30min后开始降温，同时停止通入氮气，当温度降低到400℃时向真空炉中循环通入二氧化碳，保温循环20min后继续降温到室温，制得改性氧化铝分子筛。
实施例3：
一种农业种植污水处理用滤料清洗剂的制备方法，包括以下步骤：
(1)将90份棉花秸秆粉、28份大豆淀粉和2份乙烯基三乙氧基硅烷混合均匀，在500℃氮气保护气氛炉中烧结2h，降温到180℃时，停止通入氮气，在空气中降低到室温；
(2)向步骤(1)混合物中加入50份改性氧化铝分子筛、20份活性炭、5份聚四氟乙烯、3份硅酸镁混合均匀，放入行星式球磨机中在乙醇为球磨介质下球磨40min，球磨转速为300r/min，球磨后清洗，干燥；
(3)用压力机将步骤(2)制备的混合物压制成直径为2cm、厚度为0.3cm的薄块，将薄块于160℃、0.52Mpa高温高压下定型20min，然后向薄块表面喷洒7份8％质量浓度的硫酸铜溶液，冷却到室温，干燥、粉碎；
(4)向步骤(3)制备的混合物中加入80份月桂醇硫酸钠、50份脂肪醇聚氧乙烯醚和13份碳酸氢钠，在200℃电阻炉中烧结20min，自然冷却到室温，研磨，过200目筛；
(5)将步骤(4)制备的混合物溶于1200去离子水中，向溶液中滴加盐酸至PH值在5-6之间，制得所述清洗剂。
所述步骤(2)球磨过程选用碳化硅磨球，磨球直径为8mm，磨球、磨料和乙醇的质量比为1.4：1：0.5。
所述改性氧化铝分子筛的改性方法为：
(1)将氧化铝分子筛和碳纤维、焦麻纤维、聚乳酸按照质量比为500：17：8：11混合均匀，在700℃电阻炉中保温烧结2h，自然冷却到室温；
(2)将步骤(1)制备的氧化铝分子筛和碳酸氢铵按照质量比为10：1混合均匀，在真空炉中加热到120℃，保温1h，自然冷却到室温；
(3)将步骤(2)制备的氧化铝分子筛放入5％质量浓度的醋酸溶液中浸泡40min，用去离子水清洗，干燥；
(4)将步骤(3)处理后的氧化铝分子筛在真空炉中加热到700℃，向真空炉中循环通入氮气，保温循环30min后开始降温，同时停止通入氮气，当温度降低到300℃时向真空炉中循环通入二氧化碳，保温循环20min后继续降温到室温，制得改性氧化铝分子筛。
对比例：
一种污水过滤筛清洗剂，以制备污水过滤筛清洗剂100g为例：
磷酸尿素络合物12g，乙二胺四乙酸7g，乙醇8.5g，苯甲酸单乙醇胺3g，二乙醇酰胺2.5g，松节油1g，余量为水。
一种污水过滤筛清洗剂的配制方式为：将上述比例的磷酸尿素络合物、乙二胺四乙酸、乙醇、苯甲酸单乙醇胺、二乙醇酰胺、松节油加一定量的水中，搅拌均匀即可得到污水过滤筛清洗剂。
选取污染程度为90％的种植业废水处理用滤料，将滤料平均分成4份，分别用等量的以上各实施例和对比例制备的清洗剂对其进行清洗，清洗相同时间后，对清洗效果进行检测，结果如下：
| 氨氮去除率/％ | 微生物去除率/％ | 悬浮物去除率/％ | |
| 实施例1 | 99.2 | 98.7 | 99.5 |
| 实施例2 | 99.2 | 98.6 | 99.4 |
| 实施例3 | 99.1 | 98.7 | 99.4 |
| 对比例 | 97.1 | 95.3 | 98.7 |
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (2)
1.一种农业种植污水处理用滤料清洗剂的制备方法，其特征在于，包括以下步骤：
(1)将棉花秸秆粉、大豆淀粉和乙烯基三乙氧基硅烷混合均匀，在400-600℃氮气保护气氛炉中烧结2-3h，降温到150-200℃时，停止通入氮气，在空气中降低到室温；
(2)向步骤(1)混合物中加入改性氧化铝分子筛、活性炭、聚四氟乙烯、硅酸镁混合均匀，放入行星式球磨机中在乙醇为球磨介质下球磨40min，球磨转速为300r/min，球磨后清洗，干燥；
(3)用压力机将步骤(2)制备的混合物压制成直径为2cm、厚度为0.3cm的薄块，将薄块于140-160℃、0.36-0.52Mpa高温高压下定型20min，然后向薄块表面喷洒8％质量浓度的硫酸铜溶液，冷却到室温，干燥、粉碎；
(4)向步骤(3)制备的混合物中加入月桂醇硫酸钠、脂肪醇聚氧乙烯醚和碳酸氢钠，在200-300℃电阻炉中烧结20min，自然冷却到室温，研磨，过200目筛；
(5)将步骤(4)制备的混合物溶于去离子水中，向溶液中滴加盐酸至PH值在5-6之间，制得所述清洗剂；
所述的农业种植污水处理用滤料清洗剂的制备方法，各原料按照以下重量份的比例组成：改性氧化铝分子筛50-70份、棉花秸秆粉80-100份、大豆淀粉25-30份、碳酸氢钠13-15份、活性炭20-30份、聚四氟乙烯5-7份、乙烯基三乙氧基硅烷2-3份、硅酸镁3-4份、月桂醇硫酸钠80-100份、脂肪醇聚氧乙烯醚50-60份、硫酸铜7-8份、盐酸适量、去离子水1000-1500份；
所述改性氧化铝分子筛的改性方法为：
(1)将氧化铝分子筛和碳纤维、焦麻纤维、聚乳酸混合均匀，在600-700℃电阻炉中保温烧结2-3h，自然冷却到室温；
(2)将步骤(1)制备的氧化铝分子筛和碳酸氢铵混合均匀，在真空炉中加热到120-125℃，保温1h，自然冷却到室温；
(3)将步骤(2)制备的氧化铝分子筛放入4-5％质量浓度的醋酸溶液中浸泡40-60min，用去离子水清洗，干燥；
(4)将步骤(3)处理后的氧化铝分子筛在真空炉中加热到600-700℃，向真空炉中循环通入氮气，保温循环30min后开始降温，同时停止通入氮气，当温度降低到300-400℃时向真空炉中循环通入二氧化碳，保温循环20min后继续降温到室温，制得改性氧化铝分子筛；
步骤(1)所述氧化铝分子筛和碳纤维、焦麻纤维、聚乳酸的质量比为500-600：17-19：7-8：11-13，步骤(2)所述氧化铝分子筛和碳酸氢铵的质量比为10：1。
2.根据权利要求1所述的农业种植污水处理用滤料清洗剂的制备方法，其特征在于，所述步骤(2)球磨过程选用碳化硅磨球，磨球直径为8mm，磨球、磨料和乙醇的质量比为1.4：1：0.5。
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