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Preparation process of zinc trifluoromethanesulfonate

A technology of zinc trifluoromethanesulfonate and trifluoromethanesulfonic acid, applied in the field of zinc trifluoromethanesulfonate production, can solve the problems affecting the preparation quality of zinc trifluoromethanesulfonate, affecting user recovery, efficiency and purity limitations, etc. problems, to achieve the effect of convenient recovery, improved preparation purity, and improved preparation efficiency

Inactive Publication Date: 2021-01-19
JIANGXI GUOHUA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the problems existing in the prior art, the purpose of the present invention is to provide a preparation process for zinc trifluoromethanesulfonate, which can improve the preparation efficiency and preparation purity of zinc trifluoromethanesulfonate, and avoid the residual trifluoromethanesulfonic acid. Advantages, solve the existing zinc trifluoromethanesulfonate preparation method, a large amo

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment one: carbon disulfide reacts with trifluoroiodomethane and sulfur to generate (CF 3 -S-S-CF 3 ), will (CF 3 -S-S-CF 3 ) reacts with mercury under light to obtain mercuric trifluoromethylthio, and the above-mentioned mercuric trifluoromethylsulfonate is further oxidized with an oxidant to generate trifluoromethanesulfonic acid monohydrate, and trifluoromethanesulfonic acid monohydrate is filtered to obtain trifluoromethanesulfonic acid monohydrate Methanesulfonic acid aqueous solution, add sufficient amount of zinc to 40% trifluoromethanesulfonic acid aqueous solution, heat to 50°C and reflux until the solution becomes neutral, the reaction time is 4h, the reaction produces zinc trifluoromethanesulfonate, cool Rotary evaporation of the filtrate was carried out at room temperature to obtain solid zinc trifluoromethanesulfonate with a preparation purity of 98.7%.

Embodiment 2

[0022] Embodiment two: carbon disulfide and iodotrifluoromethane and sulfur react to generate (CF 3 -S-S-CF 3 ), will (CF 3 -S-S-CF 3 ) reacts with mercury under light to obtain mercuric trifluoromethylthio, and the above-mentioned mercuric trifluoromethylsulfonate is further oxidized with an oxidant to generate trifluoromethanesulfonic acid monohydrate, and trifluoromethanesulfonic acid monohydrate is filtered to obtain trifluoromethanesulfonic acid monohydrate Methanesulfonic acid aqueous solution, add enough zinc to the trifluoromethanesulfonic acid aqueous solution of 40% concentration, heat to 75 ℃ and reflux until the solution is neutral, the reaction time is 3.5h, and the reaction generates zinc trifluoromethanesulfonate, Cool to room temperature and perform rotary evaporation of the filtrate to obtain solid zinc trifluoromethanesulfonate with a preparation purity of 99.1%.

Embodiment 3

[0023] Embodiment three: carbon disulfide and trifluoroiodomethane and sulfur reaction generate (CF 3 -S-S-CF 3 ), will (CF 3 -S-S-CF 3 ) reacts with mercury under light to obtain mercuric trifluoromethylthio, and the above-mentioned mercuric trifluoromethylsulfonate is further oxidized with an oxidant to generate trifluoromethanesulfonic acid monohydrate, and trifluoromethanesulfonic acid monohydrate is filtered to obtain trifluoromethanesulfonic acid monohydrate Methanesulfonic acid aqueous solution, add sufficient amount of zinc to the 60% concentration trifluoromethanesulfonic acid aqueous solution, heat to 100 ℃ and reflux until the solution is neutral, the reaction time is 2.5h, the reaction generates zinc trifluoromethanesulfonate, Cool to room temperature and perform rotary evaporation of the filtrate to obtain solid zinc trifluoromethanesulfonate with a preparation purity of 99.5%.

[0024] Criteria for judging: Comparing Examples 1, 2 and 3, changing the concentra...

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Abstract

The invention belongs to the field of production of zinc trifluoromethanesulfonate, and discloses a preparation process of zinc trifluoromethanesulfonate, which comprises the following raw materials:carbon disulfide, trifluoroiodomethane, sulfur, mercury, hydrogen peroxide and zinc, and comprises the following production steps: step 1, reacting carbon disulfide with trifluoroiodomethane and sulfur to generate (CF3-S-S-CF3); step 2, reacting (CF3-S-S-CF3) with mercury under illumination to obtain trifluoromethylthio mercury; 3, further oxidizing the trifluoromethylthio mercury and an oxidizingagent to generate trifluoromethanesulfonic acid monohydrate; 4, filtering the trifluoromethanesulfonic acid monohydrate to obtain a trifluoromethanesulfonic acid aqueous solution; and step 5, addingsufficient zinc into the trifluoromethanesulfonic acid aqueous solution, and heating and refluxing until the solution is neutral. Compared with an existing zinc trifluoromethanesulfonate production process, the preparation efficiency and the preparation purity of zinc trifluoromethanesulfonate can be effectively improved, the final product of zinc trifluoromethanesulfonate preparation is neutral,excessive influence on the outside is avoided, and recovery is convenient.

Description

technical field [0001] The invention relates to the technical field of zinc trifluoromethanesulfonate production, in particular to a preparation process of zinc trifluoromethanesulfonate. Background technique [0002] Zinc trifluoromethanesulfonate, white to light gray powder, easy to absorb moisture, easily soluble in water. Catalyst for the synthesis of dithioketals; preferred reagent in Koenigs-Knorr type glycosylation processes; catalyst for thioketalization reactions of ketones. [0003] The existing zinc trifluoromethanesulfonate preparation method will leave a large amount of trifluoromethanesulfonic acid after the preparation is completed, which needs to be absorbed by distillation reaction of water, phosphoric acid and carbonate, etc., which affects the recovery of users. At the same time, the preparation method The efficiency and purity of extracting zinc trifluoromethanesulfonate are limited, which affects the preparation quality of zinc trifluoromethanesulfonate...

Claims

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Application Information

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IPC IPC(8): C07C303/32C07C309/06
CPCC07C303/32C07C319/24C07C319/08C07C303/16
Inventor 陈红斌祝金玲
Owner JIANGXI GUOHUA IND CO LTD
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