Fluid method for continuous preparation of iron oxide nanoparticles

A nano-fluid technology of iron oxide, applied in the direction of iron oxide, nanotechnology for materials and surface science, iron oxide/iron hydroxide, etc., can solve the problems of poor repeatability and uneven particle size, and achieve low cost and shape Uniform appearance and high mass transfer efficiency

Active Publication Date: 2020-08-28
SOUTHEAST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems of morphology, uneven particle size and poor repeatability of iron oxide nanoparticles prepared by co-precipitation method, the present invention proposes a new method for continuous preparation of iron oxide nanoparticles in combination with fluid technology

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  • Fluid method for continuous preparation of iron oxide nanoparticles
  • Fluid method for continuous preparation of iron oxide nanoparticles
  • Fluid method for continuous preparation of iron oxide nanoparticles

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Effect test

Embodiment 1

[0036]Ferrous chloride tetrahydrate (89.5 mg) and ferric chloride hexahydrate (243.3 mg) were ultrasonically dissolved in 20 ml ultrapure water, and the coating agent citric acid monohydrate (63 mg) was ultrasonically dissolved in 10 ml ultrapure water. The above solution was mixed ultrasonically and placed in a 50 ml syringe. Set the injection rate of the reaction solution to 500 μl / min, the flow rate of ammonia gas to 3.5 sccm, and the flow rate of nitrogen gas to 14 sccm. A PTFE tube with an inner diameter of 2.2 mm and a length of 10 m was connected to the reactor and placed in an alcohol bath at 1 °C. The residence time of the reaction solution in the PTFE tube was about 3 min. The schematic diagram of the reaction device and experiment implementation is as follows: figure 1 shown. Collect the product at room temperature and pass through 20 sccm nitrogen protection, use ultrapure water to wash the sample repeatedly by ultrafiltration until the solution is neutral, and ...

Embodiment 2

[0038] Ultrasonically dissolve ferrous chloride tetrahydrate (29.8 mg) and ferric chloride hexahydrate (81.1 mg) in 20 ml ultrapure water, and ultrasonically dissolve the coating agent PSC (90 mg) in 10 ml ultrapure water middle. The above solution was mixed ultrasonically and placed in a 50 ml syringe. Set the injection rate of the reaction solution to 500 μl / min, the flow rate of ammonia gas to 3.5 sccm, and the flow rate of nitrogen gas to 14 sccm. A PTFE tube with an inner diameter of 2.2 mm and a length of 10 m was connected to the reactor and placed in an alcohol bath at 1 °C. The residence time of the reaction solution in the PTFE tube was about 3 min. Collect the product at room temperature and pass through 20 sccm nitrogen protection, use ultrapure water to wash the sample repeatedly by ultrafiltration until the solution is neutral, and obtain PSC-modified iron oxide nanoparticles with uniform particle size and morphology distribution, such as image 3 shown. The c...

Embodiment 3

[0040] Ultrasonically dissolve ferrous chloride tetrahydrate (29.8 mg) and ferric chloride hexahydrate (81.1 mg) in 30 ml ultrapure water, and place the reaction solution in a 50 ml syringe. Set the solution injection rate to 2 ml / min, the ammonia gas flow to 5 sccm, and the nitrogen gas flow to 15 sccm. A PTFE tube with an inner diameter of 2.2 mm and a length of 15 cm was connected to the reactor and placed at room temperature. The residence time of the reaction solution in the PTFE tube was about 3 s. The product was directly passed into a three-necked flask, the product was collected at room temperature and protected by 20 sccm nitrogen, and the reaction was continued to stir at 600 rpm for 1 h. After the reaction is over, use ultrapure water to wash the sample repeatedly through magnetic separation until the solution is neutral to obtain unmodified bare iron oxide nanoparticles, such as Figure 4 shown. The magnets used for magnetic separation are NdFeB magnets.

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Abstract

The invention relates to a fluid method for continuous preparation of iron oxide nanoparticles. The fluid method mainly comprises the following steps: respectively dissolving an iron salt precursor and a coating agent; mixing the obtained coating agent solution with the obtained iron salt precursor solution; injecting the mixed solution into a T-shaped channel from an inlet 2 at a first flow ratethrough a fluid device, meanwhile, inputting a mixed gas of nitrogen and ammonia gas into the T-shaped channel from the inlet 1 at a second flow speed, shearing the liquid-phase fluid by the gas phaseat a two-phase junction so as to form uniform liquid sections which are alternately distributed with the gas sections in an output pipeline, meanwhile, dissolving part of ammonia gas in the liquid phase to form an alkaline environment so as to enable the precursor to be subjected to a hydrolysis reaction, and curing the product in the pipeline; and collecting the output product, and washing the product for multiple times by using ultrapure water through an ultrafiltration or magnetic separation process to remove redundant ions, thereby obtaining the final product. The method is green and environment-friendly, is low in cost, can realize continuous and repeatable preparation of the iron oxide nanoparticles, and is suitable for industrial application.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic nanomaterials, and in particular relates to a method for continuously preparing iron oxide nanoparticles by using a fluid device. particle method. Background technique [0002] Magnetic iron oxide nanoparticles have good biocompatibility and magnetic properties, and have broad application prospects in the fields of biomedicine, environmental restoration, and electronics. For example, magnetic iron oxide nanoparticles have been used for targeted drug delivery, magnetic Resonance imaging, tumor hyperthermia, immunoassay, sewage treatment, magnetic ink printing, microwave absorption, magnetic storage devices, etc., have attracted the attention of a large number of researchers. There are many chemical methods for the synthesis of magnetic iron oxide nanoparticles, including co-precipitation method, high-temperature pyrolysis method, microemulsion method, sol-gel method, hydrothermal method, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06B82Y30/00B82Y40/00
CPCC01G49/06B82Y30/00B82Y40/00C01P2004/04C01P2004/52C01P2004/64
Inventor 顾宁毛宇孙剑飞陈博
Owner SOUTHEAST UNIV
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