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Method for recovering trifluoromethanesulfonic acid in wastewater

A technology for trifluoromethanesulfonic acid and waste water, applied in chemical instruments and methods, water/sewage multi-stage treatment, preparation of organic compounds, etc., can solve problems such as high product cost, waste water discharge, and environmental damage, and achieve a recycling method Simple and convenient, reduce environmental pollution and reduce cost

Active Publication Date: 2013-05-01
GUANGZHOU WISDOM BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As a newly developed reagent, trifluoromethanesulfonic acid has a high price. At present, trifluoromethanesulfonic acid is discharged as waste water after the reaction is completed. If it is not recycled, the cost of the product will be high, and the fluorine in it will also be destroyed. surroundings
[0005] However, in large-scale production, it is found that the viscosity of trimethylamine sulfate and other substances produced by the method of removing organic bases with concentrated sulfuric acid is very large, which seriously affects the recovery of trifluoromethanesulfonic acid.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A method for reclaiming trifluoromethanesulfonic acid in waste water, comprising the following steps:

[0038] 1) Take 1000 g of waste water containing trimethylamine trifluoromethanesulfonate in a three-necked flask, the waste water contains 20.9 g (0.1 mol) of trimethylamine trifluoromethanesulfonate, add 4 g of sodium hydroxide (0.1 mol), Stir the reaction for 10 minutes, then evaporate the water to dryness at a temperature of 80° C. and a vacuum pressure of 250 Pa to obtain 35 g of solid matter;

[0039] 2) Add 175 g of absolute ethanol to 35 g of solid matter and reflux for 2 h, filter out the insoluble matter, then cool to 5 ° C, let stand for 3 h, filter, and dry to obtain 15.1 g of sodium trifluoromethanesulfonate;

[0040] 3) Add 8.6g (0.088 mol) of concentrated sulfuric acid to 15.1 g of sodium trifluoromethanesulfonate. After dissolving, heat up to 100°C and recover under a vacuum pressure of 500 Pa to obtain 10.5g of anhydrous trifluoromethanesulfonic acid w...

Embodiment 2

[0042] A method for reclaiming trifluoromethanesulfonic acid in waste water, comprising the following steps:

[0043] 1) Take 1000 g of trifluoromethanesulfonic acid-containing wastewater in a three-necked flask, and the wastewater contains 15g (0.1 mol) of trifluoromethanesulfonic acid, add 5.6g of potassium hydroxide (0.1 mol), stir for 10 minutes, and then Evaporate to dryness at 80°C and a vacuum pressure of 250 Pa to obtain 40 g of solid matter;

[0044] 2) Add 400 g of absolute ethanol to 40 g of solid matter and reflux for 1 h, filter out the insoluble matter while it is hot, then cool to 0 ° C, let stand for 3 h, filter, and dry to obtain 13.2 g of potassium trifluoromethanesulfonate;

[0045] 3) Add 6.88g (0.07 mol) of concentrated sulfuric acid to 13.2g of potassium trifluoromethanesulfonate. After dissolving, heat up to 100°C and recover under vacuum pressure of 500 Pa to obtain 9.3g of anhydrous trifluoromethanesulfonic acid with a content of 98.3%. .

Embodiment 3

[0047] A method for reclaiming trifluoromethanesulfonic acid in waste water, comprising the following steps:

[0048] 1) Take 1000 g of waste water containing trimethylammonium trifluoromethanesulfonate in a three-necked flask, the waste water contains 20.9 g (0.1 mol) of trimethylamine trifluoromethanesulfonate, add 5.6 g of potassium hydroxide (0.1 mol), The reaction was stirred for 10 minutes, and then evaporated to dryness at a temperature of 80° C. and a vacuum pressure of 250 Pa to obtain 42 g of solid matter;

[0049] 2) Add 7 times the weight of absolute ethanol to 42g of solid matter and reflux for 1.5h, filter out the insoluble matter, then cool to 4°C, let stand for 3h, filter, and dry to obtain 13g of potassium trifluoromethanesulfonate;

[0050] Add 6.78 g (0.069 mol) of concentrated sulfuric acid to 13 g of potassium trifluoromethanesulfonate. After dissolving, heat up to 100° C. and recover under a vacuum pressure of 500 Pa to obtain 9 g of anhydrous trifluorom...

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Abstract

The invention discloses a method for recovering trifluoromethanesulfonic acid in wastewater, which comprises the following steps: adding inorganic alkali into trifluoromethanesulfonic acid-containing wastewater and reacting; then evaporating to dryness, adding ethanol and reflowing, filtrating, cooling, standing and separating out trifluoromethanesulfonic acid inorganic salt, filtrating, drying; then adding concentrated sulphuric acid into the trifluoromethanesulfonic acid inorganic salt and dissolving; and finally reducing pressure and recovering trifluoromethanesulfonic acid, wherein the trifluoromethanesulfonic acid in the wastewater exists in the form of free state or organic alkali salt. The trifluoromethanesulfonic acid recovered by the method has high purity and high productivity, and the recovery method is simple and convenient, and is suitable for large-scale industrial application; and the method provided by the invention is safe, and provides a beneficial solution method for reducing cost and environment pollution as much as possible.

Description

technical field [0001] The invention relates to a method for recovering trifluoromethanesulfonic acid in waste water, in particular to a method for recovering trifluoromethanesulfonic acid from waste water containing trifluoromethanesulfonic acid. Background technique [0002] Trifluoromethanesulfonic acid is the strongest organic acid known so far. It has strong acidity and reducing properties. It is generally used as a reagent for organic synthesis, and can also be used as a catalyst for isomerization and alkylation, so that it is widely used in medicine and chemical industry. And other industries, such as nucleosides, antibiotics, steroids, proteins, glycosides, vitamin synthesis, silicone rubber modification, etc. In particular, it is found that these three aspects are relatively broad. The first is that it is used to protect functional groups in organic synthesis, and it is a very effective methyl silylation reagent; the second is that in organic synthesis, it participa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/06C07C303/44C02F9/08
Inventor 吴世林张贵东邸维龙史志君
Owner GUANGZHOU WISDOM BIO TECH
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