Prepn process of nanometer nickel sulfide rod

A technology of nano-rods and nickel sulfide, applied in the direction of nickel sulfide, etc., can solve the problems of complex precursor preparation process, non-single reaction product, and difficult control of product shape, and achieve high yield, short reaction time, and thermal stability Good results

Inactive Publication Date: 2007-06-06
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of the precursor required by this method is complicated, the reaction product is not single, the nanorods and nanosheets cannot be effectively separated, and the product morphology is not easy to control

Method used

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  • Prepn process of nanometer nickel sulfide rod
  • Prepn process of nanometer nickel sulfide rod
  • Prepn process of nanometer nickel sulfide rod

Examples

Experimental program
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Embodiment 1

[0025] Embodiment 1, the preparation steps of nickel sulfide nanorods are: (1) preparation of nickel octane sulfonate: take 0.005molNiSO 4 ·6H 2 O was dissolved in water, weighed 0.01mol octane potassium sulfonate and dissolved in methanol, and added the nickel sulfate aqueous solution dropwise into the potassium sulfonate solution to obtain a khaki-yellow precipitate immediately. After the dropwise addition, fully stir. The resulting mixture was filtered with suction, and the filter cake was washed three times with methanol:water at a ratio of 3:1 (volume ratio), and then washed once with methanol, filtered with suction, and the filter cake was vacuum-dried for later use. The resulting product is nickel octane sulfonate. (2) Preparation of ionic liquid: methylimidazole and hexyl bromide 1:1 (molar ratio) were added to the flask, the temperature of the oil bath was slowly raised to 60°C and stirred for 5 hours, then cooled to room temperature, dissolved in distilled water, an...

Embodiment 2

[0028] Embodiment 2, the preparation steps of nickel sulfide nanorods are: (1) Preparation of nickel cetyl sulfonate: the raw material is potassium cetyl sulfonate, and the preparation method is the same as in Example 1. (2) Preparation of ionic liquid: the raw material was changed to potassium hexafluorophosphate, and the preparation method was the same as in Example 1. (3) Preparation of nickel sulfide nanorods: Add 0.03g of nickel hexadecyl sulfonate and 3mL of 1-hexyl-3-methylimidazolium hexafluorophosphate ionic liquid into a 50mL single-necked bottle, and gently stir with a magnetic stirrer. Stir to disperse nickel cetyl sulfonate evenly in the ionic liquid, put the one-necked bottle into the oil bath, and slowly heat the oil bath from room temperature to 170°C, while stirring magnetically, keep it for 5 minutes, then place the one-necked bottle After the solution is cooled to room temperature, the product is separated by centrifugation, and the separated product is wash...

Embodiment 3

[0030]Embodiment 3, the preparation steps of nickel sulfide nanorods are: (1) Preparation of nickel hexadecyl sulfonate: same as in embodiment 2. (2) The preparation method of the ionic liquid is the same as in Example 2. (3) Preparation of NiS nanorods: Add 0.03g of nickel hexadecyl sulfonate and 3mL of 1-hexyl-3-methylimidazolium hexafluorophosphate ionic liquid into a 50mL single-necked bottle, and stir gently with a magnetic stirrer , so that nickel hexadecyl sulfonate is evenly dispersed in the ionic liquid, put the one-mouth bottle into the oil bath, and slowly heat the oil bath from room temperature to 210 ° C, while magnetic stirring, keep for 30 minutes, and then take out the one-mouth bottle , after the solution was cooled to room temperature, the product was separated by centrifugation, the separated product was washed 5 times with acetone, and then dried at room temperature to obtain a shuttle-shaped nickel sulfide nanorod.

[0031] As shown in FIG. 4 , the analys...

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Abstract

The present invention relates to preparation process of nanometer nickel sulfide rod, and belongs to the field of nanometer material preparing technology. The improved preparation process includes dissolving nickel alkyl xanthate with C8-C22 straight chain or branched chain in ionic liquid, maintaining at 140-210 deg.c for 5 min to 3 hr, and separation to obtain the product. The ionic liquid consists of cation and anion, the cation is N, N'-dialkyl imidazole ion, and the cation is BF4-, PF6-, CF3COO-, C3F7COO-, CF3SO3-, C4F9SO3-, (CF3SO2)2N-, (C2F5SO2)2N-, (CF3SO2)3C-, SbF6- or AsF6- ion. The product of the process has relatively identical shape, and the process has the advantages of fast speed and environment friendship and is suitable for mass production.

Description

technical field [0001] The invention relates to a method for preparing nanometer materials, in particular to a method for preparing nickel sulfide nanorods. Background technique [0002] Nanomaterials have many excellent properties different from bulk materials, and have broad application prospects in the fields of chemistry, physics, materials and machinery. One-dimensional nanomaterials exhibit excellent properties different from those of bulk materials and nanoparticles in many aspects, and have very promising application prospects in the connection and composition of nanodevices. [0003] In recent years, room temperature ionic liquids (Room temperature ionic liquids) are being recognized and accepted as a relatively environment-friendly solvent and catalyst. Ionic liquid has no vapor pressure (non-volatile), non-combustible, good electrical conductivity, high thermal stability, and is in a liquid state in a wide temperature range. It can dissolve many organic and inorg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11
Inventor 张晟卯张春丽吴志申张治军
Owner HENAN UNIVERSITY
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