CN205074538U - Synthetic washing integrated device of zeroth order iron - Google Patents
Synthetic washing integrated device of zeroth order iron Download PDFInfo
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- CN205074538U CN205074538U CN201520836597.3U CN201520836597U CN205074538U CN 205074538 U CN205074538 U CN 205074538U CN 201520836597 U CN201520836597 U CN 201520836597U CN 205074538 U CN205074538 U CN 205074538U
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000005406 washing Methods 0.000 title claims abstract description 43
- 229910052742 iron Inorganic materials 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 24
- 230000015572 biosynthetic process Effects 0.000 claims description 21
- 239000000706 filtrate Substances 0.000 claims description 16
- 238000007789 sealing Methods 0.000 claims description 14
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims 6
- 238000001914 filtration Methods 0.000 claims 3
- 239000000376 reactant Substances 0.000 claims 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 25
- 239000007789 gas Substances 0.000 abstract description 22
- 239000007788 liquid Substances 0.000 abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 13
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 8
- 238000005070 sampling Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- 238000003756 stirring Methods 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000012279 sodium borohydride Substances 0.000 description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003032 molecular docking Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- IZUPBVBPLAPZRR-UHFFFAOYSA-N pentachlorophenol Chemical compound OC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl IZUPBVBPLAPZRR-UHFFFAOYSA-N 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- DJHGAFSJWGLOIV-UHFFFAOYSA-K Arsenate3- Chemical compound [O-][As]([O-])([O-])=O DJHGAFSJWGLOIV-UHFFFAOYSA-K 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229940000489 arsenate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003993 organochlorine pesticide Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
本实用新型公开了一种零价铁合成洗涤一体化装置，包括反应器主体、进气装置、反应液滴加装置、排气装置和洗涤装置，其中反应器主体的上部分别设有用于安装进气装置的进气标准接口、用于安装反应液滴加装置的进液标准接口、用于安装排气装置的排气标准接口和用于连接洗涤装置的排液标准接口，排气标准接口与排液标准接口为同一标准接口。本实用新型不仅能够有效持续通入氮气排尽反应室内的氧气，而且又能在氮气保护的作用下简便地对合成的零价铁进行洗涤，方便将合成的零价铁过滤在滤膜上，便于取样分析，又可有效避免零价铁的自身氧化所导致的活性降低或损失，更能方便地对合成的零价铁进行取用。
The utility model discloses an integrated device for synthesizing and washing zero-valent iron, which comprises a reactor main body, an air intake device, a reaction liquid dripping device, an exhaust device and a washing device, wherein the upper part of the reactor main body is respectively equipped with The air inlet standard interface of the gas device, the liquid inlet standard interface for installing the reaction liquid dripping device, the exhaust standard interface for installing the exhaust device, and the drain standard interface for connecting the washing device, the exhaust standard interface is the same as The drain standard interface is the same standard interface. The utility model can not only effectively and continuously feed nitrogen to exhaust the oxygen in the reaction chamber, but also can easily wash the synthesized zero-valent iron under the protection of nitrogen, and conveniently filter the synthesized zero-valent iron on the filter membrane. It is convenient for sampling and analysis, and can effectively avoid the activity reduction or loss caused by the self-oxidation of zero-valent iron, and it is more convenient to take the synthesized zero-valent iron.
Description
技术领域 technical field
本实用新型属于零价铁的合成技术领域，具体涉及一种零价铁合成洗涤一体化装置。 The utility model belongs to the technical field of synthesis of zero-valent iron, in particular to an integrated device for synthesis and washing of zero-valent iron.
背景技术 Background technique
零价铁材料成为目前环境污染修复技术中一个非常活跃的研究领域。零价铁具有较大的比表面积，粒径小，表面能大以及较高的表面活性，是一种环境友好型还原剂。近年来，零价铁能够处理多种污染物，其对于有机氯农药、五氯苯酚、杀虫剂、卤化烷烃、卤化芳香烃、多氯联苯、重金属离子、砷酸盐及铬酸盐等多种污染物均具有还原转化的作用，因此，零价铁能够用于环境污染的治理并作为一种新的污染控制技术。 Zero-valent iron materials have become a very active research field in environmental pollution remediation technology. Zero-valent iron has a large specific surface area, small particle size, large surface energy and high surface activity, and is an environmentally friendly reducing agent. In recent years, zero-valent iron has been able to treat a variety of pollutants, such as organochlorine pesticides, pentachlorophenol, pesticides, halogenated alkanes, halogenated aromatics, polychlorinated biphenyls, heavy metal ions, arsenate and chromate, etc. A variety of pollutants have the function of reduction and transformation, therefore, zero-valent iron can be used in the treatment of environmental pollution and as a new pollution control technology.
近年来，关于零价铁的合成及修饰的研究越来越多，然而零价铁粒径较小，易团聚而降低比表面积，易氧化而降低反应活性，在零价铁的合成过程中，对于零价铁的洗涤与取样过程更加繁琐，不易控制。目前，对零价铁的研究过程中对反应条件的控制方面仍存在一定的局限性，在零价铁的合成过程中，通常是在圆底烧瓶等玻璃仪器中完成，对于零价铁的洗涤与取样过程较为繁琐，不易控制。为优化零价铁的合成过程，有必要针对以上不足之处设计出一种既能方便操作，又能控制反应过程以及方便洗涤和取样的零价铁合成洗涤一体化装置。 In recent years, there have been more and more studies on the synthesis and modification of zero-valent iron. However, the particle size of zero-valent iron is small, and it is easy to agglomerate and reduce the specific surface area, and it is easy to oxidize and reduce the reactivity. During the synthesis of zero-valent iron, The washing and sampling process for zero-valent iron is more cumbersome and difficult to control. At present, there are still some limitations in the control of reaction conditions in the research process of zero-valent iron. In the synthesis process of zero-valent iron, it is usually completed in glass instruments such as round bottom flasks. For the washing of zero-valent iron The sampling process is cumbersome and difficult to control. In order to optimize the synthesis process of zero-valent iron, it is necessary to design an integrated zero-valent iron synthesis and washing device that can not only facilitate operation, but also control the reaction process and facilitate washing and sampling.
发明内容 Contents of the invention
本实用新型解决的技术问题是提供了一种结构简单且易于控制的零价铁合成洗涤一体化装置，该装置可以有效提高零价铁合成的可操作性，有效简化零价铁的洗涤工艺和取样工艺，有效避免零价铁在合成过程中被氧化，同时有效提高零价铁合成过程的可控性。 The technical problem solved by the utility model is to provide a zero-valent iron synthesis and washing integrated device with simple structure and easy control, which can effectively improve the operability of zero-valent iron synthesis, and effectively simplify the washing process and process of zero-valent iron. The sampling process can effectively prevent the zero-valent iron from being oxidized during the synthesis process, and at the same time effectively improve the controllability of the zero-valent iron synthesis process.
本实用新型为解决上述技术问题采用如下技术方案，零价铁合成洗涤一体化装置，其特征在于包括反应器主体、进气装置、反应液滴加装置、排气装置和洗涤装置，反应器主体的上部分别设有用于安装进气装置的进气标准接口、用于安装反应液滴加装置的进液标准接口、用于安装排气装置的排气标准接口和用于连接洗涤装置的排液标准接口，其中排气标准接口与排液标准接口为同一标准接口，洗涤装置通过连接管和抽滤管与排液标准接口密封，洗涤装置由上下分体结构的洗涤室和滤液室对接而成，洗涤室与滤液室之间设有滤膜，洗涤室与滤液室通过紧固连接装置连接并箍紧密封，洗涤室与连接管通过磨砂面接口密封连接。 In order to solve the above technical problems, the utility model adopts the following technical scheme, the zero-valent iron synthesis and washing integrated device is characterized in that it includes a reactor main body, an air inlet device, a reaction liquid dripping device, an exhaust device and a washing device, and the reactor main body The upper part is respectively provided with the air inlet standard interface for installing the air inlet device, the liquid inlet standard interface for installing the reaction liquid dripping device, the exhaust standard interface for installing the exhaust device and the liquid discharge for connecting the washing device Standard interface, in which the exhaust standard interface and the liquid discharge standard interface are the same standard interface, the washing device is sealed with the liquid discharge standard interface through the connecting pipe and the suction filter tube, and the washing device is formed by docking the washing chamber and the filtrate chamber of the upper and lower split structures A filter membrane is arranged between the washing chamber and the filtrate chamber, the washing chamber and the filtrate chamber are connected and tightly sealed through a fastening connection device, and the washing chamber and the connecting pipe are sealed and connected through a frosted surface interface.
进一步优选，所述的反应器主体由上下分体结构的密封盖和反应室构成，该密封盖与反应室的连接处通过磨砂面接口密封。 Further preferably, the reactor body is composed of an upper and lower split sealing cover and a reaction chamber, and the connection between the sealing cover and the reaction chamber is sealed through a frosted interface.
进一步优选，所述的进气装置包括气体管道接口，该气体管道接口的底部与进气标准接口通过磨砂面接口密封连接，气体管道接口上设有气体流量调节阀门。 Further preferably, the air inlet device includes a gas pipeline interface, the bottom of the gas pipeline interface is sealed and connected to the air inlet standard interface through a frosted surface interface, and a gas flow regulating valve is provided on the gas pipeline interface.
进一步优选，所述的反应液滴加装置包括带有刻度的恒压分液漏斗，该恒压分液漏斗的底部与进液标准接口通过磨砂面接口密封连接，恒压分液漏斗的下端设有流量控制阀门，恒压分液漏斗的上端通过磨口盖密封。 Further preferably, the reaction liquid dropping device includes a graduated constant pressure separating funnel, the bottom of the constant pressure separating funnel is sealed and connected to the liquid inlet standard interface through a frosted surface interface, and the lower end of the constant pressure separating funnel is set There is a flow control valve, and the upper end of the constant pressure separating funnel is sealed by a ground cover.
进一步优选，所述的排气装置与洗涤装置交替与反应器主体连接，反应过程中排气标准接口与排气装置密封连接，反应完成后洗涤装置通过连接管和抽滤管与排液标准接口密封连接，其中抽滤管伸入到反应器主体的底部。 Further preferably, the exhaust device and the washing device are alternately connected to the main body of the reactor. During the reaction, the exhaust standard interface is sealed and connected to the exhaust device. After the reaction is completed, the washing device is connected to the discharge standard interface through the connecting pipe and the suction filter pipe. Sealed connection, in which the suction filter tube extends into the bottom of the reactor body.
进一步优选，所述的洗涤装置滤液室的中上部设有负压接口，该负压接口与真空泵的抽气管连接。 Further preferably, a negative pressure port is provided in the middle and upper part of the filtrate chamber of the washing device, and the negative pressure port is connected with the suction pipe of the vacuum pump.
本实用新型与现有技术相比具有以下有益效果： Compared with the prior art, the utility model has the following beneficial effects:
本实用新型是一种适用于高效合成零价铁的装置，不仅适用于零价铁材料的合成，而且也能够用于零价铁的各种修饰研究。本实用新型不仅能够有效持续通入氮气排尽反应室内的氧气，而且又能在氮气保护的作用下简便地对合成的零价铁进行洗涤，方便将合成的零价铁过滤在滤膜上，便于取样分析，又可有效避免零价铁的自身氧化所导致的活性降低或损失，更能方便地对合成的零价铁进行取用。 The utility model is a device suitable for efficiently synthesizing zero-valent iron, which is not only suitable for the synthesis of zero-valent iron materials, but also can be used for various modification studies of zero-valent iron. The utility model can not only effectively and continuously feed nitrogen to exhaust the oxygen in the reaction chamber, but also can easily wash the synthesized zero-valent iron under the protection of nitrogen, and conveniently filter the synthesized zero-valent iron on the filter membrane. It is convenient for sampling and analysis, and can effectively avoid the activity reduction or loss caused by the self-oxidation of zero-valent iron, and it is more convenient to take the synthesized zero-valent iron.
附图说明 Description of drawings
图1是本实用新型的结构示意图。 Fig. 1 is the structural representation of the utility model.
图面说明：1、密封盖，2、反应室，3、气体管道接口，4、气体流量控制阀门，5、磨口盖，6、恒压分液漏斗，7、流量控制阀门，8、连接管，9、抽滤管，10、洗涤室，11、滤膜，12、紧固连接装置，13、负压接口，14、滤液室。 Drawing description: 1. Sealing cover, 2. Reaction chamber, 3. Gas pipeline interface, 4. Gas flow control valve, 5. Ground cover, 6. Constant pressure separating funnel, 7. Flow control valve, 8. Connection Tube, 9, suction filter tube, 10, washing chamber, 11, filter membrane, 12, fastening connection device, 13, negative pressure interface, 14, filtrate chamber.
具体实施方式 detailed description
结合附图详细描述本实用新型的具体内容。如图1所示，零价铁合成洗涤一体化装置，包括反应器主体、进气装置、反应液滴加装置、排气装置和洗涤装置，反应器主体的上部分别设有用于安装进气装置的进气标准接口、用于安装反应液滴加装置的进液标准接口、用于安装排气装置的排气标准接口和用于连接洗涤装置的排液标准接口，其中排气标准接口与排液标准接口为同一标准接口，洗涤装置通过连接管8和抽滤管9与排液标准接口密封连接，洗涤装置由上下分体结构的洗涤室10和滤液室14对接而成，洗涤室10与滤液室14之间设有滤膜11，洗涤室10与滤液室14通过紧固连接装置12连接并箍紧密封，洗涤室10与连接管8通过磨砂面接口密封连接。 The specific content of the utility model is described in detail in conjunction with the accompanying drawings. As shown in Figure 1, the zero-valent iron synthesis and washing integrated device includes a reactor main body, an air intake device, a reaction liquid dripping device, an exhaust device and a washing device. The upper part of the reactor main body is respectively equipped with an air intake device The air inlet standard interface, the liquid inlet standard interface for installing the reaction liquid dripping device, the exhaust standard interface for installing the exhaust device, and the drain standard interface for connecting the washing device, where the exhaust standard interface is the same as the exhaust The liquid standard interface is the same standard interface, and the washing device is sealed and connected with the liquid discharge standard interface through the connecting pipe 8 and the suction filter tube 9. The washing device is formed by docking the washing chamber 10 and the filtrate chamber 14 of the upper and lower split structures. A filter membrane 11 is arranged between the filtrate chambers 14 , the washing chamber 10 and the filtrate chamber 14 are connected and tightly sealed through a fastening connection device 12 , and the washing chamber 10 and the connecting pipe 8 are sealed and connected through a frosted interface.
所述的反应器主体由上下分体结构的密封盖1和反应室2构成，该密封盖1与反应室2的连接处通过磨砂面接口密封，反应室1优选采用派克玻璃材质的圆筒形容器，反应室1的体积为2-3L。所述的进气装置包括气体管道接口3，该气体管道接口3的底部与进气标准接口通过磨砂面接口密封连接，气体管道接口3上设有气体流量调节阀门4，通过控制气体流量调节阀门4的大小能够控制通入氮气的气体量。所述的反应液滴加装置为带有刻度的恒压分液漏斗6，该恒压分液漏斗6的底部与进液标准接口通过磨砂面接口密封连接，恒压分液漏斗6的下端设有流量控制阀门7，恒压分液漏斗6的上端通过磨口盖5密封，通过流量控制阀门7调节恒压分液漏斗6中反应原料的滴加速度，进而控制反应速率，还可以通过进液标准接口通入洗涤液。所述的排气装置与洗涤装置交替与反应器主体连接，反应过程中排气标准接口与排气装置密封连接，反应完成后洗涤装置通过连接管8和抽滤管9与排液标准接口密封连接，其中抽滤管9伸入到反应器主体的底部。所述的洗涤装置的滤液室14中上部设有负压接口13，该负压接口13与真空泵的抽气管连接，能够更好地对合成的零价铁进行抽滤，滤液室14优选为派克玻璃材质的圆筒形容器，滤液室14的体积为1-2L。 The main body of the reactor is composed of a sealing cover 1 and a reaction chamber 2 with an upper and lower split structure. The connection between the sealing cover 1 and the reaction chamber 2 is sealed by a frosted surface interface. The reaction chamber 1 is preferably a cylinder made of Parker glass. device, the volume of the reaction chamber 1 is 2-3L. The air intake device includes a gas pipeline interface 3, the bottom of the gas pipeline interface 3 is sealed and connected to the air intake standard interface through a frosted surface interface, and the gas pipeline interface 3 is provided with a gas flow regulating valve 4, which is adjusted by controlling the gas flow. The size of 4 can control the gas amount that feeds nitrogen. The reaction liquid dripping device is a constant pressure separatory funnel 6 with a scale, the bottom of the constant pressure separatory funnel 6 is sealed and connected to the liquid inlet standard interface through a frosted surface interface, and the lower end of the constant pressure separatory funnel 6 is set There is a flow control valve 7, and the upper end of the constant pressure separating funnel 6 is sealed by the ground cover 5, and the dropping speed of the reaction raw materials in the constant pressure separating funnel 6 is adjusted through the flow control valve 7, thereby controlling the reaction rate. The standard interface leads to the washing liquid. The exhaust device and the washing device are alternately connected to the main body of the reactor. During the reaction process, the exhaust standard interface is sealed and connected to the exhaust device. After the reaction is completed, the washing device is sealed with the drain standard interface through the connecting pipe 8 and the suction filter pipe 9. Connection, wherein suction filter pipe 9 stretches into the bottom of the reactor main body. The upper part of the filtrate chamber 14 of the washing device is provided with a negative pressure interface 13, which is connected with the suction pipe of the vacuum pump, and can better filter the synthesized zero-valent iron. The filtrate chamber 14 is preferably Parker A cylindrical container made of glass, the volume of the filtrate chamber 14 is 1-2L.
下面通过3个应用实例来具体描述本实用新型的具体应用。 The specific application of the utility model is described in detail below through 3 application examples.
实施例1 Example 1
如图1所示，将该装置置于磁力搅拌器上，打开密封盖，将0.7993gFeSO4·7H2O、40mL蒸馏水和0.05g聚乙二醇加入到反应室内，然后将密封盖通过磨砂面接口与反应室密封，安装进气装置即气体管道接口，并将该气体管道接口与氮气瓶连接，打开气体流量控制阀门，不断通入氮气，经排气装置排出，置换反应室内的空气。在剧烈搅拌下，通过反应液滴加装置的恒压分液漏斗滴加用稀HNO3调节pH=3的0.1mol/L的NaBH4溶液200mL，通过恒压分液漏斗的流量控制阀门控制反应液的滴加速度，在反应室内进行纳米零价铁的化学合成反应，滴加完毕后，继续搅拌反应2-4h。然后拆下排气装置，将洗涤装置通过连接管和抽滤管密封连接到反应器主体上，将合成纳米零价铁和反应后的液体抽到洗涤装置内，合成的纳米零价铁过滤在滤膜上，反应液抽滤到滤液室内。然后通过进液标准接口多次加入蒸馏水和无水乙醇进行洗涤冲洗，去除残余的NaBH4等杂质，整个制备合成过程都在氮气保护下进行。最后将合成的干净的纳米零价铁过滤在滤膜上，便于取用。 As shown in Figure 1, place the device on a magnetic stirrer, open the sealing cover, add 0.7993g FeSO 4 7H 2 O, 40mL distilled water and 0.05g polyethylene glycol into the reaction chamber, and then put the sealing cover through the frosted surface The interface is sealed with the reaction chamber, the air inlet device is installed, that is, the gas pipeline interface, and the gas pipeline interface is connected to the nitrogen cylinder, the gas flow control valve is opened, nitrogen is continuously introduced, and it is discharged through the exhaust device to replace the air in the reaction chamber. Under vigorous stirring, drop 200mL of 0.1mol/L NaBH4 solution adjusted to pH= 3 with dilute HNO3 through the constant pressure separating funnel of the reaction solution dropping device, and control the reaction through the flow control valve of the constant pressure separating funnel The drop rate of the liquid is increased, and the chemical synthesis reaction of nanometer zero-valent iron is carried out in the reaction chamber. After the dropwise addition is completed, the stirring reaction is continued for 2-4 hours. Then remove the exhaust device, connect the washing device to the main body of the reactor through the connecting pipe and the suction filter tube, pump the synthesized nano-zero-valent iron and the reacted liquid into the washing device, and filter the synthesized nano-zero-valent iron in the On the filter membrane, the reaction solution is suction filtered into the filtrate chamber. Then add distilled water and absolute ethanol several times through the liquid inlet standard interface for washing and flushing to remove residual NaBH 4 and other impurities. The entire preparation and synthesis process is carried out under nitrogen protection. Finally, the synthesized clean nanometer zero-valent iron is filtered on the filter membrane for easy access.
实施例2 Example 2
如图1所示，将该装置置于磁力搅拌器上，打开密封盖，将0.7993gFeSO4·7H2O、40mL蒸馏水、分子筛1.0g和0.05g聚乙二醇加入到反应室内，然后将密封盖通过磨砂面接口与反应室密封，安装进气装置即气体管道接口，并将气体管道接口与氮气瓶连接，打开气体流量控制阀门，不断通入氮气，经排气装置排出，置换反应室内的空气。在剧烈搅拌下，通过反应液滴加装置的恒压分液漏斗滴加用稀HNO3调节pH=3的0.1mol/L的NaBH4溶液200mL，通过恒压分液漏斗的流量控制阀门控制反应液的滴加速度，在反应室内进行纳米零价铁的化学合成反应，滴加完毕后，继续搅拌反应2-4h。以下操作同应用实例1。 As shown in Figure 1, place the device on a magnetic stirrer, open the sealed cover, add 0.7993g FeSO 4 7H 2 O, 40mL distilled water, 1.0g molecular sieve and 0.05g polyethylene glycol into the reaction chamber, and then put the sealed The cover is sealed with the reaction chamber through the frosted surface interface, the air inlet device is installed, that is, the gas pipeline interface, and the gas pipeline interface is connected to the nitrogen cylinder, the gas flow control valve is opened, nitrogen is continuously introduced, and it is discharged through the exhaust device to replace the nitrogen in the reaction chamber. Air. Under vigorous stirring, drop 200mL of 0.1mol/L NaBH4 solution adjusted to pH= 3 with dilute HNO3 through the constant pressure separating funnel of the reaction solution dropping device, and control the reaction through the flow control valve of the constant pressure separating funnel The drop rate of the liquid is increased, and the chemical synthesis reaction of nanometer zero-valent iron is carried out in the reaction chamber. After the dropwise addition is completed, the stirring reaction is continued for 2-4 hours. The following operations are the same as application example 1.
实施例3 Example 3
如图1所示，将该装置置于磁力搅拌器上，打开密封盖，将0.4996gFeSO4·7H2O、40mL蒸馏水和0.05g聚乙二醇加入到反应室内，然后将密封盖通过磨砂面接口与反应室密封，然后安装进气装置即气体管道接口，并将气体管道接口与氮气瓶连接，打开气体流量控制阀门，不断通入氮气，经排气装置排出，置换反应室内的空气。在剧烈搅拌下，通过反应液滴加装置的恒压分液漏斗滴加用稀HNO3调节pH=3的0.1mol/L的NaBH4溶液200mL，通过恒压分液漏斗的流量控制阀门控制反应液的滴加速度，在反应室内进行纳米零价铁的化学合成反应，滴加完毕后，继续搅拌反应2-4h。以下操作同应用实例1。 As shown in Figure 1, place the device on a magnetic stirrer, open the sealing cover, add 0.4996g FeSO 4 7H 2 O, 40mL distilled water and 0.05g polyethylene glycol into the reaction chamber, and then put the sealing cover through the frosted surface The interface is sealed with the reaction chamber, and then the air inlet device is installed, that is, the gas pipeline interface, and the gas pipeline interface is connected to the nitrogen cylinder, the gas flow control valve is opened, nitrogen is continuously introduced, and it is discharged through the exhaust device to replace the air in the reaction chamber. Under vigorous stirring, drop 200mL of 0.1mol/L NaBH4 solution adjusted to pH= 3 with dilute HNO3 through the constant pressure separating funnel of the reaction solution dropping device, and control the reaction through the flow control valve of the constant pressure separating funnel The drop rate of the liquid is increased, and the chemical synthesis reaction of nanometer zero-valent iron is carried out in the reaction chamber. After the dropwise addition is completed, the stirring reaction is continued for 2-4 hours. The following operations are the same as application example 1.
以上显示和描述了本实用新型的基本原理，主要特征和优点，在不脱离本实用新型精神和范围的前提下，本实用新型还有各种变化和改进，这些变化和改进都落入要求保护的本实用新型的范围。 The basic principles, main features and advantages of the present utility model have been shown and described above. On the premise of not departing from the spirit and scope of the present utility model, the present utility model also has various changes and improvements, and these changes and improvements all fall into the claims. The scope of the utility model.
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| CN111230137A (en) * | 2020-01-15 | 2020-06-05 | 上海海事大学 | Integrated reaction device for preventing nano zero-valent iron from being oxidized and use method thereof |
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