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A fluid method for the 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 The effect of uniform appearance and uniform particle size distribution

Active Publication Date: 2022-03-11
SOUTHEAST UNIV
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  • Summary
  • 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

Method used

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  • A fluid method for the continuous preparation of iron oxide nanoparticles
  • A fluid method for the continuous preparation of iron oxide nanoparticles
  • A fluid method for the continuous preparation of iron oxide nanoparticles

Examples

Experimental program
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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 experimental 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, an...

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 50ml 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 ce...

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 that can be used for continuous preparation of iron oxide nanoparticles, which mainly includes the following steps: separately dissolving the iron salt precursor and the coating agent; mixing the coating agent solution and the iron salt precursor solution; passing through a fluid device The mixed solution is injected into the T-shaped channel from the inlet 2 at the first flow rate, and the mixed gas of nitrogen and ammonia is input into the T-shaped channel from the inlet 1 at the second flow rate, and the liquid phase fluid is sheared by the gas phase at the confluence of the two phases. In the output pipeline, a uniform liquid section is formed that is distributed alternately with the gas section. At the same time, the ammonia gas is partially dissolved in the liquid phase to form an alkaline environment to hydrolyze the precursor, and the product is matured in the pipeline; the output product is collected. The final product is obtained by washing the product several times with ultrapure water to remove excess ions by means of ultrafiltration or magnetic separation. The invention is green and environment-friendly, has low cost and can realize continuous and repeatable preparation of 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 Patents(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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