Unlock instant, AI-driven research and patent intelligence for your innovation.

Comprehensive treatment method for kettle residues in preparation of trifluoromethanesulfonic acid

A technology of trifluoromethanesulfonic acid and trifluoromethanesulfonic anhydride, applied in chemical instruments and methods, preparation of organic compounds, phosphorus compounds, etc., can solve the problems of difficult separation, high boiling range, solid and liquid wastes that cannot be treated and other problems, to achieve the effect of solving environmental protection problems and simple operation

Active Publication Date: 2021-12-31
PERIC SPECIAL GASES CO LTD
View PDF10 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In industry, potassium trifluoromethanesulfonate and concentrated sulfuric acid are generally used as raw materials to prepare product trifluoromethanesulfonic acid, while the residue in the still is potassium sulfate, excess sulfuric acid, a small amount of unfractionated trifluoromethanesulfonic acid and bound water, which Several kinds of kettle residues are mixed together, and the boiling range is relatively high. Generally, the method of vacuum distillation makes it difficult to separate them, and solid and liquid wastes cannot be treated.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A kind of comprehensive processing method of still residue in the preparation of trifluoromethanesulfonic acid, described still residue is the residue potassium sulfate (mass fraction 30%), excess sulfuric acid (mass fraction is 60%), unfractionated trifluoromethanesulfonic acid (mass fraction is 5%) and bound water (mass fraction is 5%), and the method steps include:

[0017] (1) Put the residue of the kettle into the reaction kettle, then add phosphorus pentoxide at 30°C, stir and react under normal pressure for 10h, then distill and recover under reduced pressure at -0.05MPa, (40-60)°C to obtain trifluoro Methanesulfonic anhydride;

[0018] (2) Cool down the reactor to 40°C and then add potassium hydroxide to carry out neutralization reaction. After pH = 7, the reaction ends, solid-liquid separation, and after the solid is dried, a mixture of potassium phosphate (phosphate fertilizer) and potassium sulfate (potassium fertilizer) is obtained. fertilizer.

[0019] Th...

Embodiment 2

[0026] A kind of comprehensive processing method of still residue in the preparation of trifluoromethanesulfonic acid, described still residue is the residue potassium sulfate (mass fraction 30%), excess sulfuric acid (mass fraction is 60%), unfractionated trifluoromethanesulfonic acid (mass fraction is 5%) and bound water (mass fraction is 5%), and the method steps include:

[0027] (1) Put the residue of the kettle into the reaction kettle, then add phosphorus pentoxide at 10°C, stir and react under normal pressure for 4h, then distill and recover under reduced pressure at -0.09MPa, (20-50)°C to obtain trifluoro Methanesulfonic anhydride;

[0028] (2) After cooling down to 30°C in the reaction kettle, add potassium carbonate to carry out neutralization reaction. After pH=6, the reaction ends, solid-liquid separation, and after the solid is dried, a mixed fertilizer of potassium phosphate (phosphate fertilizer) and potassium sulfate (potassium fertilizer) is obtained. .

[...

Embodiment 3

[0036] A kind of comprehensive processing method of still residue in the preparation of trifluoromethanesulfonic acid, described still residue is the residue potassium sulfate (mass fraction 30%), excess sulfuric acid (mass fraction is 60%), unfractionated trifluoromethanesulfonic acid (mass fraction is 5%) and bound water (mass fraction is 5%), and the method steps include:

[0037] (1) Put the residue of the kettle into the reaction kettle, then add phosphorus pentoxide at 60°C, stir and react under normal pressure for 20h, then distill and recover under reduced pressure at -0.03MPa, (60-100)°C to obtain trifluoro Methanesulfonic anhydride;

[0038] (2) Cool down the reactor to 60°C and then add potassium bicarbonate for neutralization reaction. After pH = 6, the reaction ends, solid-liquid separation, and after the solid is dried, a mixture of potassium phosphate (phosphate fertilizer) and potassium sulfate (potassium fertilizer) is obtained. fertilizer.

[0039] The mate...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a comprehensive treatment method for kettle residues in trifluoromethanesulfonic acid preparation, and belongs to the technical field of chemical engineering. The method comprises the following steps: by taking kettle residues generated in preparation of trifluoromethanesulfonic acid as a raw material, firstly adding phosphorus pentoxide into a reaction kettle for reaction, then carrying out reduced pressure distillation and recovery to obtain a product trifluoromethanesulfonic anhydride, then cooling, then adding a certain amount of potassium hydroxide, potassium carbonate or potassium bicarbonate for neutralization, by controlling a reaction endpoint, centrifugally separating and drying to obtain a product potassium phosphate and potassium sulfate mixed fertilizer. The method is simple to operate, can fully utilize kettle residues to produce high-added-value products, solves the problem of environmental protection, and also can bring certain economic benefits.

Description

technical field [0001] The invention relates to a comprehensive treatment method for still residues in the preparation of trifluoromethanesulfonic acid, which belongs to the technical field of chemical industry. Background technique [0002] In industry, potassium trifluoromethanesulfonate and concentrated sulfuric acid are generally used as raw materials to prepare product trifluoromethanesulfonic acid, while the residue in the still is potassium sulfate, excess sulfuric acid, a small amount of unfractionated trifluoromethanesulfonic acid and bound water, which Several kinds of kettle residues are mixed together, and the boiling range is relatively high. Generally, the method of vacuum distillation makes it difficult to separate them, and solid and liquid wastes cannot be treated. Contents of the invention [0003] In view of this, the object of the present invention is to provide a kind of comprehensive processing method to the still residue in the preparation of trifluo...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C05G1/06C01B25/30C01D5/00C07C309/06C07C303/00
CPCC05B7/00C01B25/30C01D5/00C07C303/00C07C309/06C05D1/02
Inventor 吕灵华罗建志户帅帅何成旷军李柄缘吕随强张帅袁瑞玲
Owner PERIC SPECIAL GASES CO LTD