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Solvothermal preparation method of regular-octahedral calcium sulfide particles

An octahedral and solvothermal technology, applied in the direction of magnesium/calcium/strontium/barium sulfide/polysulfide, etc., can solve the problems of harmful gas leakage, low purity of CaS, high reaction temperature, etc., and achieve uniform scale, high purity, Simple operation effect

Active Publication Date: 2018-01-05
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The calcium sulfide prepared by the above method is mostly spherical, the required reaction temperature is high, it is easy to cause harmful gas leakage, the operation is relatively complicated, and the purity of the generated CaS is low

Method used

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  • Solvothermal preparation method of regular-octahedral calcium sulfide particles
  • Solvothermal preparation method of regular-octahedral calcium sulfide particles
  • Solvothermal preparation method of regular-octahedral calcium sulfide particles

Examples

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Effect test

Embodiment example 1

[0041] (1) Prepare the solution: take 0.222g of calcium chloride through a 100-mesh sieve and place it in a conical flask, add 20ml of ethylenediamine to form the first solution; feed nitrogen into the conical flask, drain the air, and let it stand stand-by;

[0042] (2) Add chelating agent: add 0.606g of L-cysteine ​​and 0.204g of EDTA respectively in the first solution, while constantly stirring, Ca 2+ Chelate with a chelating agent to obtain a second solution; feed nitrogen gas, and sonicate for 30 minutes at a power of 300W;

[0043] (3) Preparation of reaction solution: Add 0.064 g of sulfur element and 0.4 ml of hydrazine hydrate monohydrate into a conical flask containing 60 ml of ethylenediamine to obtain a third solution; then, sonicate for 30 min under 300 W ultrasonic conditions.

[0044] (4) Reaction: Pour the second solution and the third solution into a 100ml polytetrafluoroethylene lining at the same time, place the lining in the iron body at 180° C. for 72 hou...

comparative example 1

[0048] (1) Preparation of solution: Dissolve 0.222g of calcium chloride in 20ml of ethylenediamine; then pass nitrogen gas to isolate the contact with air; place the solution in an ultrasonic generator and ultrasonicate for 30min under the condition of 300W ultrasonic power to form a mixed solution.

[0049] (2) Preparation of reaction solution: Mix 0.064 g of sulfur element and 60 ml of ethylenediamine in a conical flask, then pass nitrogen gas again, and sonicate for 30 min under 300 W ultrasonic conditions.

[0050] (3) Reaction: Pour the above solution into a hydrothermal reaction kettle and keep it warm for 20 hours at 180° C., so as to observe the development process of CaS.

[0051] (4) Isolate the product: cool down the above solution naturally, open the reaction kettle by hand, collect the supernatant for later use, filter through absolute ethanol, wash, and dry to obtain a solid powder.

[0052] Scanning electron micrographs of CaS powders are shown in figure 2 , i...

comparative example 2

[0054] (1) Prepare the solution: add 20ml of ethylenediamine to the conical flask of 0.222g of calcium chloride crossing 100 mesh sieves; then, feed nitrogen to isolate the contact with the air; Ultrasonic 30min under the condition of 300W ultrasonic power, so that calcium chloride is uniformly dispersed in the solvent.

[0055] (2) Preparation of reaction solution: add 0.064g sulfur element to the conical flask containing 60ml ethylenediamine, the color of the solution changes, indicating that the sulfur element is converted into S 2- , Ultrasonic 30min under 300W ultrasonic conditions.

[0056] (3) Reaction: Pour the above two solutions into a hydrothermal reaction kettle, and keep the temperature at 180°C for 72 hours to make the reaction fully proceed.

[0057] (4) Isolate the product: cool down the above solution naturally, pour the upper layer of ethylenediamine solution into a waste liquid bottle for recycling; filter and wash with absolute ethanol, and then dry it in ...

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Abstract

The invention discloses a solvothermal preparation method of regular-octahedral calcium sulfide particles. The solvothermal preparation method comprises that regular-octahedral CaS particles with uniform sizes are prepared from sublimed sulfur as a sulfur source, calcium chloride as a calcium source, ethylenediamine as a reaction solvent, L-cysteine and ethylenediaminetetraacetic acid (EDTA) as chelating agents and a hydrazine monohydrate as a reductant through a solvothermal method. Through change of concentrations of the chelating agents and reductant in a reactor, Ca<2+> and S<2-> release rates are controlled so that the dissolution-recrystallization rate of the CaS particles is controlled. Through adjusting reaction time, CaS spherical particles are recrystallized to form regular-octahedral particles. The solvothermal preparation method has the characteristics of simple operation, mild conditions, safety and environmental friendliness, is suitable for large-scale production and hasa wide industrial prospect.

Description

technical field [0001] The invention belongs to the technical field of preparation of alkaline earth metal sulfide CaS, in particular to a method for solvothermally preparing regular octahedral CaS particles. Background technique [0002] At present, the method of preparing CaS is mainly solid-solid reaction method or gas-solid reaction method, such as: carbon reduces calcium sulfate at high temperature to obtain CaS particles; sulfur sources such as hydrogen sulfide or carbon disulfide react with calcium salt in gas form to prepare CaS particles . The calcium sulfide prepared by the above method is mostly spherical, the required reaction temperature is relatively high, and harmful gas leakage is easily caused, the operation is relatively complicated, and the purity of the generated CaS is low. At the same time, S in CaS 2- It is reductive and easy to be oxidized, and the exposed surface of the regular octahedral CaS is the {111} crystal face group, and the {111} crystal f...

Claims

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Application Information

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IPC IPC(8): C01B17/42
Inventor 田红景昌晶许静文
Owner QINGDAO UNIV OF SCI & TECH
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