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KMnF3 nanowire and preparation method thereof

A nanowire, oil-soluble technology, applied in the field of preparation of KMnF3 nanowires, can solve the problems of being unsuitable for large-scale production, difficult to elute the solvent, uneven reaction, etc., and achieve suitable for large-scale production, uniform product morphology, The effect of the simple method of synthesis

Inactive Publication Date: 2017-05-31
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the size distribution of the particles synthesized by this method is not easy to control, and the solvent is not easy to elute
[0006] In summary, the currently prepared KMnF 3 The morphology of nanocrystals has cubic phase particles and needles, and KMnF with a one-dimensional nanowire structure has not yet appeared. 3
Moreover, the existing preparation methods generally have shortcomings such as uneven reaction, unsuitability for large-scale production, and poor control of reaction particle size.

Method used

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  • KMnF3 nanowire and preparation method thereof
  • KMnF3 nanowire and preparation method thereof
  • KMnF3 nanowire and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] This embodiment prepares KMnF according to the following steps 3 Nanowires:

[0024] a. Add 6.00g Mn(CH 3 COOH) 2 and 28.00g of sodium oleate were dissolved in a mixture of 38mL of distilled water, 70mL of n-hexane and 28mL of ethanol, stirred evenly, then stirred and kept at 60°C for 9h. The resulting reaction solution was moved to a separatory funnel, washed with water three times, and the wine-red solution in the upper layer was the prepared manganese oleate solution, which was vacuum-dried to obtain manganese oleate;

[0025] b. Add 0.21g manganese oleate to the mixed solution of 4.5mL oleic acid, 4mL oleylamine and 13mL octadecene, stir evenly; then vacuumize at 100°C for 8min to remove water, then lower to room temperature to obtain a mixed reaction liquid;

[0026] c. Add 7mL of methanol solution with 0.25g of KF into the mixed reaction solution and stir evenly; first heat to 75°C and keep warm for 15mim to remove methanol; then raise the temperature to 105°C...

Embodiment 2

[0031] This embodiment prepares KMnF according to the following steps 3 Nanowires:

[0032] a, 5.00gMnCl 2 and 20.00g of sodium oleate were dissolved in a mixture of 34mL of distilled water, 59mL of n-hexane and 25mL of ethanol, stirred evenly, then stirred and kept at 50°C for 8h. The resulting reaction solution was transferred to a separatory funnel, washed with water three times, and the wine-red solution in the upper layer was the prepared manganese oleate solution, which was vacuum-dried to obtain manganese oleate.

[0033] b. Add 0.09g manganese oleate into the mixed solution of 2mL oleic acid, 3mL oleylamine and 9mL octadecene, and stir evenly. Vacuum at 90°C for 5 minutes to remove water, then lower to room temperature to obtain a mixed reaction solution.

[0034] c. Add 3mL of methanol solution with 0.08g of KF into the mixed reaction solution and stir evenly; first heat to 50°C and keep warm for 10mim to remove methanol; then raise the temperature to 90°C, vacuumi...

Embodiment 3

[0038] This embodiment prepares KMnF according to the following steps 3 Nanowires:

[0039] a. Add 9.00gMn(NO 3 ) 2 and 35.00g of sodium oleate were dissolved in a mixture of 45mL of distilled water, 83mL of n-hexane and 38mL of ethanol, stirred evenly, then stirred and kept at 90°C for 12h. The resulting reaction solution was transferred to a separatory funnel, washed with water three times, and the wine-red solution in the upper layer was the prepared manganese oleate solution, which was vacuum-dried to obtain manganese oleate.

[0040] b. Add 0.243g manganese oleate into the mixed solution of 5mL oleic acid, 7mL oleylamine and 15mL octadecene, and stir evenly. Vacuum at 110° C. for 10 minutes to remove water, and then lower to room temperature to obtain a mixed reaction solution.

[0041] c. Add 8mL methanol solution with 0.296g KF into the mixed reaction solution, stir evenly; first heat to 80°C, keep warm for 30mim to remove methanol; then raise the temperature to 110...

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Abstract

The invention discloses a KMnF3 nanowire and a preparation method thereof,. The KMnF3 nanowire is characterized in that one-dimension oil-soluble KMnF3 nanowire is prepared by mixing manganese oleate, oleic acid, oleylamine and octadecene according to a certain proportion and reacting under a condition of excessive potassium fluoride. According to the invention, the one-dimension oil-soluble KMnF3 nanowire is synthesized by the high-temperature oil phase method for the first time, and water-soluble KMnF3 nanowire is obtained after high molecular surface modification, has a longitudinal molar relaxation rate r1 of 4-6 mM<-1>s<-1>, and is a good T1 magnetic resonance imaging (MRI) contrast agent.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation and relates to a KMnF 3 Methods of preparing nanowires. Background technique [0002] The properties of nanomaterials are closely related to their size, structure and morphology. The relaxation performance of magnetic resonance contrast agents is closely related to the shape and size of nanomaterials. The commonly used T 1 Type contrast agents are Gd-DTPA, MnO, Mn 3 o 4 Wait. Among them, the divalent manganese ion has 5 unpaired electrons that can shorten T 1 The relaxation time of , which can be used as the magnetic resonance T 1 contrast agent. Mn-based contrast agents have attracted extensive attention due to their good biocompatibility and relatively high relaxivity. QUR 3 It is a new type of manganese-based contrast agent developed in recent years, which has good biocompatibility and high longitudinal relaxation efficiency. Currently KMnF 3 The synthesis of mainly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/06B82Y40/00
CPCC01G45/006C01G45/06C01P2002/72C01P2002/86C01P2004/04C01P2004/16
Inventor 钱海生郝梨娜刘坤陆杨
Owner HEFEI UNIV OF TECH
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