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Method for preparing tetrasulfur tetranitride by ammoniation of disulfur dichloride

A technology of disulfur dichloride and tetrasulfur nitride, which is applied in the fields of chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of complex reaction, low yield and poor safety of the preparation method, and achieve The effect of small equipment investment, less three wastes, and simple process flow

Inactive Publication Date: 2018-04-17
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current preparation method has complex reactions, poor safety and low yield

Method used

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  • Method for preparing tetrasulfur tetranitride by ammoniation of disulfur dichloride

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0025] Take 5ml S 2 Cl 2 In a 250ml two-necked flask, dilute to 100ml with anhydrous ether. In order to reduce solvent loss, place the flask in an ice-water bath, feed ammonia gas into one end, and connect a spherical condenser tube to the other end. The gas outlet of the spherical condenser tube communicates with the ammonia gas inlet. Under strong magnetic stirring, circulate ammonia gas at 1000ml / min for about 35min (if the reaction raw material S 2 Cl 2 Doubling the time for feeding ammonia gas is extended by 1.3 to 1.6 times), and during the reaction, it is observed that the liquid in the reactor changes from light yellow to brown, and obvious solids are produced. Add 10ml of anhydrous diethyl ether every 10 minutes of reaction. When the reactant in the reactor is a completely uniform golden-red liquid-solid mixture, take a part of the mixture and dilute it 5 times with distilled water to test its pH. If pH>8, the reaction can be stopped.

[0026] The liquid-solid mixt...

example 2

[0031] Take 10ml S 2 Cl 2 In a 250ml two-necked flask, dilute to 150ml with anhydrous ether. In order to reduce solvent loss, place the flask in an ice-water bath, feed ammonia gas into one end, and connect a spherical condenser tube to the other end. The gas outlet of the spherical condenser tube communicates with the ammonia gas inlet. Under strong magnetic stirring, ammonia gas was circulated at 1100ml / / min for 1h. During the reaction, it was observed that the liquid in the reactor changed from light yellow to brown, and there were obvious solids that continued to react. Add 10ml of anhydrous diethyl ether every 15 minutes of reaction. When the reactant in the reactor is a completely uniform golden-red liquid-solid mixture, take a part of the mixture and dilute it 5 times with distilled water to test its pH. If pH>8, the reaction can be stopped.

[0032] The liquid-solid mixture obtained in the reaction was separated, and the obtained solid was rinsed with anhydrous ether ...

example 3

[0037] Take 15ml S 2 Cl 2 In a 500ml two-necked flask, dilute to 200ml with anhydrous ether. In order to reduce solvent loss, place the flask in an ice-water bath, feed ammonia gas at one end, and connect a spherical condenser tube at the other end. The gas outlet of the spherical condenser tube communicates with the ammonia gas inlet. Under strong magnetic stirring, ammonia gas was circulated at 1200ml / / min for 1.2h. During the reaction, it was observed that the liquid in the reactor changed from light yellow to brown at the beginning, and there were obvious solids. 20ml of anhydrous diethyl ether. When the reactant in the reactor is a completely uniform golden-red liquid-solid mixture, take part of the mixture and dilute it 5 times with distilled water to test its pH, and the reaction can be stopped when pH>8. According to experience, the reaction is complete in about 1.2h.

[0038] The liquid-solid mixture obtained by the reaction was separated by suction filtration with...

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Abstract

The invention discloses a method for preparing tetrasulfur tetranitride by ammoniation of disulfur dichloride. The reaction is performed in an ice-water bath, and is mainly characterized in that disulfur dichloride is diluted by taking absolute ether as a solvent, dried ammonia gas is introduced into the disulfur dichloride dilute solution in a circulating feeding manner for reaction, and a crudeproduct produced after reaction is completed is subjected to suction filtration to separate out the liquid phase and the solid phase. After the liquid phase is dried by distillation, insoluble substances are rinsed and filtered out with dichloromethane, and the obtained liquid is dried by spinning to obtain a solid; furthermore, the solid obtained by reaction is dissolved in water and filtered, soxhlet extraction is performed on the solid obtained after filtering with dioxane, and the extraction solution is cooled, filtered and dried by distillation to obtain a solid. Furthermore, the solids obtained in two times are combined, and recrystallization is performed by using methylbenzene, so as to obtain tetrasulfur tetranitride crystal. The method is simple in reaction, recyclable in solvent,green, economical and reasonable, and relatively high in yield.

Description

technical field [0001] The invention belongs to the field of inorganic chemical industry, and in particular relates to a method for preparing tetrasulfur tetranitride by ammonating disulfide dichloride. Background technique [0002] Tetrasulfur tetranitride is an important inorganic chemical intermediate. Its structure and bonding are special. It is the most important raw material for preparing other compounds containing S-N bonds. It can also be used as an important intermediate of insulating gas. Very good application prospects. [0003] Tetrasulfur tetranitride can be prepared from disulfur dichloride and ammonia gas in carbon tetrachloride solvent, and S can also be prepared at 170°C 2 Cl 2 Vapor passing through pelleted NH 4 Cl made. However, the current preparation method has complex reactions, poor safety and low yield. For this reason, the present invention optimizes the preparation process to prepare tetrasulfur tetranitride in a simple, green and efficient man...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/0865
Inventor 彭敏于萍王宝山罗运柏
Owner WUHAN UNIV
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