CN112044405B - 一种医药废水处理剂及其制备方法 - Google Patents
一种医药废水处理剂及其制备方法 Download PDFInfo
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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 abstract description 68
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/0222—Compounds of Mn, Re
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- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
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- B01J23/34—Manganese
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开了一种医药废水处理剂,以重量份计,包括以下组分:高岭石纳米管改性含钛硅凝胶10‑15份,硫酸铝5‑8份,聚丙烯酰胺10‑20份;聚合氯化铝铁5‑15份;多孔陶粒负载锰铈复合物5‑10份。本发明还公开了该医药废水处理剂的制备方法。该方法操作简单,成本低,制得的医药废水处理剂无毒、环保,能很好的除去医药废水中的有机污染物,对水体无二次污染。
Description
技术领域:
本发明涉及医药废水处理领域,具体涉及一种医药废水处理剂及其制备方法。
背景技术:
在过去的几十年里,药品消费一直在增加,每年有超过3000种商业上可获得的药物进入市场,主要是由于医疗保健行业快速发展,世界人口的增加,科学和研究的进步,慢性病的高患病率和预期寿命的增加。医药废水主要来源于制药和医疗产生的废水。医药废水处理技术包括物理过程(气浮法,混凝沉淀法等),化学过程(化学氧化法,催化氧化法等),生物处理技术和非常规处理技术。这些技术在有效性和成本方面都有所不同,每种技术都有自己的技术优点和局限。
气浮是分离固液和液液的有效方法。高度分散的微气泡用作附接于废水中的悬浮污染物的载体,从而使浮力大于重力和阻力时,允许污染物漂浮在水面上以形成泡沫,然后安装装置,用于从水表面进行泡沫固化。凝结沉淀过程是一种从废水中去除悬浮固体和胶体的分离方法。它通常用于预处理和前处理。将凝结剂添加到废水中以破坏胶体的稳定性,并将废水中的胶体和细悬浮液组合成具有可分离性的旋转体。该技术操作简便,维护成本低,去除率通常可达50%以上,应用非常广泛。化学氧化法主要包括臭氧、UV、芬顿法等,臭氧是一种环境友好的氧化剂,常被自来水公司和污水处理厂用来消毒和增强污水处理效果。通过氧化剂的氧化作用,使难降解的有机物转化为易降解有机物,或将有机物彻底氧化为二氧化碳和水的方法。生物处理技术主要是利用微生物的代谢作用分解和转化废水中的有机污染物,来达到净化水体的目的。
上述方法中常常用到的是化学处理发,这种处理方式处理医药废水较为彻底,处理后能够达到排放标准。该方法处理医药废水的关键在于开发出一种能有效除去医药废水中有机污染物的处理剂。
发明内容:
本发明要解决的技术问题是,针对现有技术的不足,提供一种医药废水处理剂及其制备方法,该方法操作简单,成本低,制得的医药废水处理剂无毒、环保,能很好的除去医药废水中的有机污染物,对水体无二次污染。
为更好的解决上述技术问题,本发明采用以下技术方案:
一种医药废水处理剂,以重量份计,包括以下组分:
高岭石纳米管改性含钛硅凝胶10-15份,
硫酸铝5-8份,聚丙烯酰胺10-20份;
聚合氯化铝铁5-15份;
多孔陶粒负载锰铈复合物5-10份。
为更好的解决上述技术问题,本发明采用以下技术方案:
一种医药废水处理剂,包括以下步骤:
(1)将高岭石粉末分散于DMSO溶液中,快速搅拌10-20h,之后离心处理,固体采用甲醇洗涤多次后重新分散于CTAB的溶液中,继续搅拌20-30h,之后超声辐射处理,制得高岭石纳米管;将钛源和硅源溶于无水乙醇中,然后加入高岭石纳米管,并滴加去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将粉煤灰、果壳、粘土、高岭土、碳酸锰、碳酸铈、水混合制得球形坯料,然后烘干后在680-710℃下进行烧结处理;制得多孔陶粒负载锰铈复合物;
(3)将高岭石纳米管改性含钛硅凝胶、多孔陶粒负载锰铈复合物、硫酸铝、聚丙烯酰胺、聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
作为上述技术方案的优选,步骤(1)中,所述搅拌的转速为800-1500rpm。
作为上述技术方案的优选,步骤(1)中,所述超声辐射处理的条件为400-500W下处理10-15min。
作为上述技术方案的优选,步骤(1)中,所述高岭石粉末、CTAB的质量比为1:(0.15-0.35)。
作为上述技术方案的优选,步骤(1)中;所述钛源为钛酸四丁酯;所述硅源为正硅酸乙酯;所述钛源、所述硅源、所述高岭石纳米管的用量比为1mol、1mol、10g。
作为上述技术方案的优选,步骤(2)中,所述粉煤灰、果壳、粘土、高岭土、碳酸锰、碳酸铈、水的质量比为5:(1-3):3:5:(1-2):(1-2):(3-5)。
作为上述技术方案的优选,步骤(2)中,所述烧结处理的条件为:首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min。
由于采用上述技术方案,本发明具有以下有益效果:
本发明制得的医药废水处理剂包括高岭石纳米管改性含钛硅凝胶、硫酸铝、聚丙烯酰胺;聚合氯化铝铁、多孔陶粒负载锰铈复合物,高岭石纳米管具有较大的比表面积,其与钛硅凝胶形成的空间网络结构互穿交联,稳定性更好,吸附性能更大;多孔陶粒具有很强的吸附性,其负载了锰铈作为活性层,具有好好的热稳定性,可作为催化剂催化医药废水中有机污染物的讲解,提高污染物的去处理;硫酸铝、聚丙烯酰胺;聚合氯化铝铁作为混合沉淀剂可与医药废水中的有机污染物发生络合聚沉。
本发明首先以DMSO和甲醇以甲氧基的形式插入到高岭石的片层间;然后采用CTAB进行修饰;在转化过程之后,高岭石薄片转变为具有片状结构的纳米卷;制得的高岭石纳米管具有多孔结构,其表面具有较多的吸附位点,将其加入到钛源和硅源的混合溶液中,搅拌水解,高岭石纳米管交叉分散在硅、钛水解物形成的三维空间网络结构中,超临界干燥后,制得具有互穿多通道高岭石纳米管改性含钛硅凝胶材料,其比表面积大,吸附性能好;本发明以粉煤灰、果壳、粘土、高岭土、碳酸锰、碳酸铈、水为原料,合理控制制备工艺,制得多孔陶粒负载锰铈复合物具有较多的多孔结构,吸附能力大,且有一定的催化活性。本发明制得的医药废水处理剂稳定性好,用于水处理时效果好,无毒、环保,对水体无二次污染。
具体实施方式:
下面通过实施例对本发明进一步说明,实施例只用于解释本发明,不会对本发明构成任何的限定。
实施例1
(1)将1g高岭石粉末分散于DMSO溶液中,800rpm下快速搅拌10h,之后离心处理,固体采用甲醇洗涤多次后重新分散于含有0.15gCTAB的溶液中,1000rpm下继续搅拌20h,之后在400W下超声辐射处理10min,制得高岭石纳米管;将1mol钛酸四丁酯和1mol正硅酸乙酯溶于100ml无水乙醇中,然后加入10g高岭石纳米管,并滴加1ml去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将10g粉煤灰、2g果壳、6g粘土、10g高岭土、2g碳酸锰、2g碳酸铈、6g水混合制得球形坯料,然后烘干后,首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min,制得多孔陶粒负载锰铈复合物;
(3)以重量份计,将10份高岭石纳米管改性含钛硅凝胶、5份多孔陶粒负载锰铈复合物、5份硫酸铝、10份聚丙烯酰胺、5份聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
实施例2
(1)将1g高岭石粉末分散于DMSO溶液中,1000rpm下快速搅拌12h,之后离心处理,固体采用甲醇洗涤多次后重新分散于含有0.2gCTAB的溶液中,1100rpm下继续搅拌20h,之后在400W下超声辐射处理10min,制得高岭石纳米管;将1mol钛酸四丁酯和1mol正硅酸乙酯溶于100ml无水乙醇中,然后加入10g高岭石纳米管,并滴加1ml去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将10g粉煤灰、6g果壳、6g粘土、10g高岭土、4g碳酸锰、2g碳酸铈、6g水混合制得球形坯料,然后烘干后,首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min,制得多孔陶粒负载锰铈复合物;
(3)以重量份计,将15份高岭石纳米管改性含钛硅凝胶、10份多孔陶粒负载锰铈复合物、8份硫酸铝、20份聚丙烯酰胺、15份聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
实施例3
(1)将1g高岭石粉末分散于DMSO溶液中,1300rpm下快速搅拌12h,之后离心处理,固体采用甲醇洗涤多次后重新分散于含有0.2gCTAB的溶液中,1300rpm下继续搅拌22h,之后在500W下超声辐射处理15min,制得高岭石纳米管;将1mol钛酸四丁酯和1mol正硅酸乙酯溶于100ml无水乙醇中,然后加入10g高岭石纳米管,并滴加1ml去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将10g粉煤灰、3g果壳、6g粘土、10g高岭土、2.5g碳酸锰、2.5g碳酸铈、7g水混合制得球形坯料,然后烘干后,首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min,制得多孔陶粒负载锰铈复合物;
(3)以重量份计,将11份高岭石纳米管改性含钛硅凝胶、6份多孔陶粒负载锰铈复合物、6份硫酸铝、12份聚丙烯酰胺、7份聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
实施例4
(1)将1g高岭石粉末分散于DMSO溶液中,1300rpm下快速搅拌15h,之后离心处理,固体采用甲醇洗涤多次后重新分散于含有0.25gCTAB的溶液中,1500rpm下继续搅拌25h,之后在400W下超声辐射处理15min,制得高岭石纳米管;将1mol钛酸四丁酯和1mol正硅酸乙酯溶于100ml无水乙醇中,然后加入10g高岭石纳米管,并滴加1ml去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将10g粉煤灰、4g果壳、6g粘土、10g高岭土、3g碳酸锰、3g碳酸铈、8g水混合制得球形坯料,然后烘干后,首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min,制得多孔陶粒负载锰铈复合物;
(3)以重量份计,将12份高岭石纳米管改性含钛硅凝胶、7份多孔陶粒负载锰铈复合物、7份硫酸铝、15份聚丙烯酰胺、7份聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
实施例5
(1)将1g高岭石粉末分散于DMSO溶液中,800rpm下快速搅拌20h,之后离心处理,固体采用甲醇洗涤多次后重新分散于含有0.25gCTAB的溶液中,1400rpm下继续搅拌25h,之后在500W下超声辐射处理15min,制得高岭石纳米管;将1mol钛酸四丁酯和1mol正硅酸乙酯溶于100ml无水乙醇中,然后加入10g高岭石纳米管,并滴加1ml去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将10g粉煤灰、5g果壳、6g粘土、10g高岭土、4g碳酸锰、3g碳酸铈、8g水混合制得球形坯料,然后烘干后,首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min,制得多孔陶粒负载锰铈复合物;
(3)以重量份计,将14份高岭石纳米管改性含钛硅凝胶、8份多孔陶粒负载锰铈复合物、7.5份硫酸铝、15份聚丙烯酰胺、15份聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
实施例6
(1)将1g高岭石粉末分散于DMSO溶液中,1300rpm下快速搅拌15h,之后离心处理,固体采用甲醇洗涤多次后重新分散于含有0.35gCTAB的溶液中,1500rpm下继续搅拌25h,之后在500W下超声辐射处理15min,制得高岭石纳米管;将1mol钛酸四丁酯和1mol正硅酸乙酯溶于100ml无水乙醇中,然后加入10g高岭石纳米管,并滴加1ml去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将10g粉煤灰、6g果壳、6g粘土、10g高岭土、3g碳酸锰、4g碳酸铈、9g水混合制得球形坯料,然后烘干后,首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min,制得多孔陶粒负载锰铈复合物;
(3)以重量份计,将13份高岭石纳米管改性含钛硅凝胶、8份多孔陶粒负载锰铈复合物、6份硫酸铝、18份聚丙烯酰胺、13份聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
将上述制得的医药废水处理剂用于医药废水处理时的效果如下,其中,对比例为未处理的医药废水。
TOC,% | COD,% | 氮去除率,% | SS去除率,% | |
实施例1 | 93.5 | 97.9 | 98.5 | 99.2 |
实施例2 | 94.9 | 98.3 | 98.8 | 99.3 |
实施例3 | 95.2 | 98.2 | 98.5 | 99.5 |
实施例4 | 94.5 | 98.5 | 98.3 | 99.3 |
实施例5 | 94.9 | 98.2 | 98.2 | 99.2 |
实施例6 | 95.3 | 98.3 | 98.6 | 99.4 |
从上述测试结果可以看出,本发明制得的医药废水处理剂用于医药废水处理时效果好,对水体无二次污染。
虽然已经对本发明的具体实施方案进行了描述,但是本发明的许多其他形式和改变对本领域技术人员而言是显而易见的。应理解所附权利要求和本发明通常涵盖本发明真实精神和范围内的所有这些明显的形式和改变。
Claims (7)
1.一种医药废水处理剂,其特征在于,以重量份计,包括以下组分:
高岭石纳米管改性含钛硅凝胶10-15份,
硫酸铝5-8份,聚丙烯酰胺10-20份;
聚合氯化铝铁5-15份;
多孔陶粒负载锰铈复合物5-10份;
其制备方法包括以下步骤:
(1)将高岭石粉末分散于DMSO溶液中,快速搅拌10-20h,之后离心处理,固体采用甲醇洗涤多次后重新分散于CTAB的溶液中,继续搅拌20-30h,之后超声辐射处理,制得高岭石纳米管;将钛源和硅源溶于无水乙醇中,然后加入高岭石纳米管,并滴加去离子水,超声条件下水解,然后滴加0.1mol/L盐酸溶液,超临界干燥处理,制得高岭石纳米管改性含钛硅凝胶;
(2)将粉煤灰、果壳、粘土、高岭土、碳酸锰、碳酸铈、水混合制得球形坯料,然后烘干后在680-710℃下进行烧结处理;制得多孔陶粒负载锰铈复合物;
(3)将高岭石纳米管改性含钛硅凝胶、多孔陶粒负载锰铈复合物、硫酸铝、聚丙烯酰胺、聚合氯化铝铁混合研磨处理,制得医药废水处理剂。
2.根据权利要求1所述的一种医药废水处理剂,其特征在于,步骤(1)中,所述搅拌的转速为800-1500rpm。
3.根据权利要求1所述的一种医药废水处理剂,其特征在于,步骤(1)中,所述超声辐射处理的条件为400-500W下处理10-15min。
4.根据权利要求1所述的一种医药废水处理剂,其特征在于,步骤(1)中,所述高岭石粉末、CTAB的质量比为1:(0.15-0.35)。
5.根据权利要求1所述的一种医药废水处理剂,其特征在于,步骤(1)中;所述钛源为钛酸四丁酯;所述硅源为正硅酸乙酯;所述钛源、所述硅源、所述高岭石纳米管的用量比为1mol、1mol、10g。
6.根据权利要求1所述的一种医药废水处理剂,其特征在于,步骤(2)中,所述粉煤灰、果壳、粘土、高岭土、碳酸锰、碳酸铈、水的质量比为5:(1-3):3:5:(1-2):(1-2):(3-5)。
7.根据权利要求1所述的一种医药废水处理剂,其特征在于,步骤(2)中,所述烧结处理的条件为:首先以3℃/min的升温速率升温至400℃保温10min,然后以10℃/min的升温速率升温至700℃,保温20min。
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