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Method for preparing mercury sulfide nanoparticles through dripping reflux

A technology of nanoparticles and mercury sulfide, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of complex synthesis process, serious environmental pollution, narrow application range, etc., and achieve uniform product particle size, simple process, low cost effect

Inactive Publication Date: 2015-05-06
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The commonly used hydrothermal reaction requires high temperature and high cost; the template method needs to find a suitable template, and after the reaction, the mold needs to be removed; the above methods have the disadvantages of relatively complicated synthesis process, difficult conditions to control, serious environmental pollution, and narrow application range.

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  • Method for preparing mercury sulfide nanoparticles through dripping reflux

Examples

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Embodiment 1

[0022] A method for preparing mercuric sulfide nanoparticles by dropwise reflux, comprising the following steps:

[0023] Step 1, take mercury source mercuric chloride 2.7151g, dissolve in water and be mixed with the mercuric chloride aqueous solution that is 18% by mass percentage, standby; Acetamide aqueous solution, standby;

[0024] Step 2. Transfer the thioacetamide aqueous solution obtained in step 1 to a three-necked flask, place it in a magnetically stirred water bath reflux device and heat it. The water bath heating temperature is 80 ° C, and then mix the mercuric chloride aqueous solution according to the chemical method while stirring. The amount of the metering relationship is controlled and the rate of addition is 1ml / min and slowly added dropwise to the three-necked flask. The stirring rate is 300 r / min. The two solutions are mixed with black precipitates. After the addition is completed, continue to stir and reflux for 0.5h. After the reflux is completed, the o...

Embodiment 2

[0026] A method for preparing mercuric sulfide nanoparticles by dropwise reflux, comprising the following steps:

[0027] Step 1, get mercuric nitrate raw material, dissolve in water and be mixed with the mercuric nitrate aqueous solution of 18% by mass percentage, standby; Get thioacetamide raw material, be mixed with water and be mixed with the thioacetamide aqueous solution of 5% by mass percentage, standby;

[0028] Step 2, transfer the mercuric nitrate aqueous solution obtained in step 1 to a three-necked flask, place it in a magnetically stirred oil bath reflux device for heating, the oil bath heating temperature is 80°C, and then stir the thioacetamide aqueous solution according to The amount of stoichiometric relationship is controlled and the rate of addition is 3ml / min and slowly added dropwise to the three-necked flask. The stirring rate is 800 r / min. The two solutions are mixed with black precipitates. After the addition is completed, continue to stir and reflux for...

Embodiment 3

[0030] A method for preparing mercuric sulfide nanoparticles by dropwise reflux, comprising the following steps:

[0031] Step 1, take 1.3575 g of mercuric chloride, dissolve it in water to prepare a 9.0% mercuric chloride aqueous solution, and set aside; get 0.3756 g of thioacetamide raw material, dissolve it in water to prepare 2.5% thioacetamide aqueous solution, spare;

[0032] Step 2. Transfer the thioacetamide aqueous solution obtained in step 1 to a three-necked flask, place it in a magnetically stirred water bath reflux device and heat it. The water bath heating temperature is 75° C. The amount of the metering relationship is controlled and the dropping rate is 2ml / min and slowly added dropwise to the three-necked flask. The stirring rate is 400 r / min. The two solutions are mixed with black precipitates. After the addition is completed, continue to stir and reflux for 1h, and then After the completion, the obtained mixed solution is centrifuged, the speed of the centr...

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Abstract

The invention discloses a method for preparing mercury sulfide nanoparticles through dripping reflux. The method comprises the following steps: step 1, taking mercury source raw materials, dissolving the mercury source raw materials in water to prepare mercury source aqueous solution for later use, taking thiacetamide raw materials, and dissolving the thiacetamide raw materials in water to prepare thiacetamide aqueous solution for later use; step 2, transferring one of the mercury source aqueous solution and thiacetamide aqueous solution into a three-necked flask, heating the solution in a magnetic stirring heating reflux device, stirring, slowly dripping the other solution into the three-necked flask according to the amount of the stoichiometric relationship, mixing the two solutions, generating black precipitates, further stirring and refluxing after the dripping operation is finished, performing centrifugal separation on the obtained mixed solution after the refluxing operation is finished, washing the precipitates, and performing vacuum drying, thereby obtaining the mercury sulfide nanoparticles. The method disclosed by the invention has the advantages of low synthetic temperature, simple process, easily controlled conditions, low cost, pollution avoidance, wide application range, uniform reactant dispersion and uniform product particle size.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, and in particular relates to a method for preparing mercury sulfide nanoparticles by dropping and refluxing. Background technique [0002] Nanomaterials have basic characteristics such as quantum size effect, small size effect, surface effect and macroscopic quantum tunneling effect. These basic characteristics make nanomaterials have many potential physical and chemical properties different from conventional materials, thus arousing people's strong interest in developing and utilizing nanomaterials. Due to its high electron mobility, low band gap, and significant pyroelectric and infrared photoconductive effects, HgS has shown broad application prospects in infrared device materials. In view of the toxicity of mercury, the research of nano-mercury sulfide is relatively Zinc and cadmium sulfide are much less. At present, the methods for preparing nano-HgS mainly include ultrason...

Claims

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Application Information

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IPC IPC(8): C01G13/00B82Y30/00
Inventor 张晓宇刘新芳李冠峰李荣芳张永花
Owner HENAN UNIV OF SCI & TECH