CN113717338A - 一种微通道反器连续生产有机絮凝剂的方法 - Google Patents
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Abstract
本发明提供一种微通道反器连续生产有机絮凝剂的方法,涉及有机絮凝剂领域,包括如下步骤:S1.按一定比例量取双氰胺、氯化铵、改性剂、甲醛,将量取的氯化铵、甲醛分别按照6:4的比例分为两份;S2.将双氰胺、改性剂及60%氯化铵加热溶于60%的甲醛溶液中,通过计量泵将混合液与水输入第一微通道反应器的第一混合区得到第一混合产物,进行一次保温反应;S3.将S1中剩余的40%氯化铵、甲醛加入到第一次保温后的第一混合产物中,形成第二混合产物,将第二混合产物通入第二微通道反应容器进行二次保温反应,一段时间后得到双氰胺‑甲醛树脂,具有环保、高效、节能、操作安全的特点。
Description
技术领域
本发明涉及有机絮凝剂领域,尤其涉及一种微通道反器连续生产有机絮凝剂的方法。
背景技术
絮凝法是我国目前处理废水最常用的方法,具有操作简单方便、成本低廉和处理效率高等特点,高效的絮凝脱色剂是絮凝法的关键。众所周知,废水中的悬浮颗粒在水介质中大多带负电荷,带有正电荷的絮凝剂与水中带负电荷的悬浮颗粒相互靠近后,使胶体颗粒处于脱稳状态,从而实现污水絮凝的目的。这种方法能够显著的降低污水的浊度和色度,并且一部分絮凝剂还可以有效的处理污水中的重金属离子、微生物以及有机质等。常用的絮凝剂按照其化学成分可分为四大类:无机絮凝剂、有机絮凝剂、微生物絮凝剂、复合絮凝剂。
专利号为CN108996646B公开了一种聚硅酸铝钙海藻酸钠复合絮凝剂的制备方法,包括以下步骤:配制浓度为0.150.50mol/L的硅酸钠溶液,并调节硅酸钠溶液的pH,经过活化处理得到淡蓝色聚硅酸溶液;在聚硅酸溶液中加入0.30.8mol/L的铝盐和0.61.0mol/L的钙盐,经过活化处理,制备得到聚硅酸铝钙絮凝剂;将经过预处理的海藻酸钠溶液加入到制备好的聚硅酸铝钙絮凝剂中,水浴搅拌,静置熟化,得到聚硅酸铝钙海藻酸钠复合絮凝剂。本发明将海藻酸钠与聚硅酸铝钙复合制备的无机天然有机复合絮凝剂,兼具无机絮凝剂与天然大分子有机絮凝剂的优点,制备方法操作简单,原料易得,成本低廉,无毒环保可生物降解,可广泛应用于处理生活用水与工业废水。
无机絮凝剂虽然生产成本低,同时也是现在污水处理最常见的絮凝剂,但是存在二次污染,处理后的水不能达标排放。微生物絮凝剂可生物降解,但是培养成本高,对环境要求高,最重要的是稳定性差,容易失活。
发明内容
本发明的目的在于提供一种微通道反器连续生产有机絮凝剂的方法,以解决上述技术问题。
本发明为解决上述技术问题,采用以下技术方案来实现:一种微通道反器连续生产有机絮凝剂的方法,其特征在于:包括如下步骤:
S1.按一定比例量取双氰胺、氯化铵、改性剂、甲醛,将量取的氯化铵、甲醛分别按照6:4的比例分为两份;
S2.将双氰胺、改性剂及60%氯化铵加热溶于60%的甲醛溶液中,通过计量泵将混合液与水输入第一微通道反应器的第一混合区得到第一混合产物,进行一次保温反应;
S3.将S1中剩余的40%氯化铵、甲醛加入到第一次保温后的第一混合产物中,形成第二混合产物,将第二混合产物通入第二微通道反应容器进行二次保温反应,一段时间后得到双氰胺-甲醛树脂。
优选的,所述S1中双氰胺、氯化铵、改性剂、甲醛的量取质量比为1:1:0.5:2。
优选的,所述改性剂为尿素。
优选的,所述S2中第一混合产物反应加热采用水浴升温,水浴升温过程中搅拌,到35℃后停止水浴升温,依靠反应中的热量升温到45℃,第一混合产物保温反应时长为30min。
优选的,S3中控制温度缓慢上升到85℃,保温反应时长为3.5h。
优选的,所述第一混合产物在第一微通道反应器中的流量为20-50g/min,第一微通道反应器长度为10-50m。
优选的,所述第二混合产物在微通道内的流速为40-60g/min,第二微通道反应器的长度为5-20m。
本发明的有益效果是:
1、采用微通道反应器与现有的常规釜式反应器相比,该工艺反应时间大大缩短,而且传质传热均匀,无放大效应,收率与釜式反应相比有一定的提高,更重要的该工艺持液体积小,提高了工艺的安全性和可操作性;
2、氯化铵有利于双氰胺与甲醛缩聚,氯化铵既可以作为催化剂,又参加了反应,一方面是因为铵盐酸性不强,含量便于控制,另一方面可以提供铵离子增加脱色剂主体上附着的—NH 3+数量,增加聚合物分子质量和电荷密度,聚合物分子和胶粒形成的絮体更易沉降,因此可达到脱色除浊的效果;
3、尿素和双氰胺的分子结构相似,都含有氨基,可与甲醛发生加成和聚合反应,尿素与甲醛反应生成的反应物活性很高,极易和其他含有氨基的酰胺化合物及其羟甲基化合物反应而共缩聚,有利于线型大分子聚合物生成,相对分子质量增加,因此絮凝剂的粘度和固含量都得到提高。
附图说明
图1为本发明的流程图;
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及附图,进一步阐述本发明,但下述实施例仅仅为本发明的优选实施例,并非全部。基于实施方式中的实施例,本领域技术人员在没有做出创造性劳动的前提下所获得其它实施例,都属于本发明的保护范围。
以下实施例所用第一微通道反应器的内径为4mm,长度为15m,第二微通道反应器的内径为4mm,长度为20m。
实施例1
如图1所示流程,将双氰胺:氯化铵:尿素:甲醛为1:1:0.5:2的比例称量,将双氰胺、尿素、60%甲醛和60%氯化铵加人到250mL安装有回流冷凝管的三颈烧瓶中,持续搅拌,水浴加热到35℃停止加热,观察到反应开始,并伴有放热现象,依靠自身反应热升至45℃左右,此为反应的第一阶段,30min后加入剩下的40%醛和氯化铵,控制温度缓慢上升到85℃,反应3.5h,即可得到双氰胺-甲醛聚合物,固含量为69%。
实施例2
按双氰胺:氯化铵:尿素:甲醛为1:1:0.5:2的比例称取,将双氰胺、称取的60%氯化铵、尿素加热溶于60%的甲醛溶液中,得到混合溶液;
通过计量泵将混合液与水输入微通道反应器的第一混合区混合得到得第一混合物料,混合后通入第一微通道反应器中进行一次保温反应,温度控制在35℃~45℃;
将剩余40%氯化铵加热溶于甲醛溶液在第二混合区混合后,与第一步保温反应后的混合液通入第二微通道反应器中进行二次保温反应,温度控制在80℃~85℃,反应结束后得所述双氰胺-甲醛树脂产品,固含量为71%。
对比实施例1与实施例2,采用微通道反应器与现有的常规釜式反应器相比,该工艺反应时间大大缩短,而且传质传热均匀,无放大效应,收率与釜式反应相比有一定的提高;更重要的该工艺持液体积小,提高了工艺的安全性和可操作性。
以上显示和描述了本发明的基本原理、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仅为本发明的优选例,并不用来限制本发明,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 (7)
1.一种微通道反器连续生产有机絮凝剂的方法,其特征在于:包括如下步骤:
S1.按一定比例量取双氰胺、氯化铵、改性剂、甲醛,将量取的氯化铵、甲醛分别按照6:4的比例分为两份;
S2.将双氰胺、改性剂及60%氯化铵加热溶于60%的甲醛溶液中,通过计量泵将混合液与水输入第一微通道反应器的第一混合区得到第一混合产物,进行一次保温反应;
S3.将S1中剩余的40%氯化铵、甲醛加入到第一次保温后的第一混合产物中,形成第二混合产物,将第二混合产物通入第二微通道反应容器进行二次保温反应,一段时间后得到双氰胺-甲醛树脂。
2.根据权利要求1所述的一种微通道反器连续生产有机絮凝剂的方法,其特征在于:所述S1中双氰胺、氯化铵、改性剂、甲醛的量取质量比为1:1:0.5:2。
3.根据权利要求2所述的一种微通道反器连续生产有机絮凝剂的方法,其特征在于:所述改性剂为尿素。
4.根据权利要求1所述的一种微通道反器连续生产有机絮凝剂的方法,其特征在于:所述S2中第一混合产物反应加热采用水浴升温,水浴升温过程中搅拌,到35℃后停止水浴升温,依靠反应中的热量升温到45℃,第一混合产物保温反应时长为30min。
5.根据权利要求1所述的一种微通道反器连续生产有机絮凝剂的方法,其特征在于:S3中控制温度缓慢上升到85℃,保温反应时长为3.5h。
6.根据权利要求1所述的一种微通道反器连续生产有机絮凝剂的方法,其特征在于:所述第一混合产物在第一微通道反应器中的流量为20-50g/min,第一微通道反应器长度为10-50m。
7.根据权利要求1所述的一种微通道反器连续生产有机絮凝剂的方法,其特征在于:所述第二混合产物在微通道内的流速为40-60g/min,第二微通道反应器的长度为5-20m。
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