Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Cyanuric fluoride preparation method

A technology of cyanuric fluoride and fluorine reaction, which is applied in the direction of organic chemistry, can solve the problems of strong corrosion of equipment, low product yield, high energy consumption of solvent recovery, etc., and achieve strong corrosion of equipment, high energy consumption, Simple operation effect

Active Publication Date: 2018-04-27
JIANGXI NORMAL UNIV
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the existing defects in the existing method for preparing cyanuric cyanuric fluoride, such as strong corrosion of equipment, high energy consumption for solvent recovery, low product yield due to side reactions easily occurring under high temperature conditions, and increased difficulty in waste salt treatment. The purpose of the present invention is to It is to provide a method for preparing cyanuric fluoride with mild reaction conditions, strong selectivity and high yield. The method is low in cost, green and environmentally friendly, and is conducive to industrial production

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Cyanuric fluoride preparation method
  • Cyanuric fluoride preparation method
  • Cyanuric fluoride preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a dry reaction vessel, add 1,3,5-trichloro-s-triazine (185g, 1mol) and tetrabutylammonium fluoride (861g, 3.3mol), anhydrous dimethyl sulfoxide (390g, 5.0mol) . The reaction was stirred at 50°C for 6 hours, (TCL followed the reaction). The reaction device was changed into a distillation device, vacuum distillation, the reduced pressure was 0.012 MPa, and 124.2 grams of colorless liquid with a boiling point of about 70° C. was collected. The content of the product measured by GC was 99.2%, and the yield was 92%. Under low temperature conditions, cyanuric fluoride is stored in containers made of polytetrafluoroethylene.

Embodiment 2

[0030] In a dry reaction vessel, add 1,3,5-trichloro-s-triazine (370g, 2mol) and tetrabutylammonium fluoride (1.722kg, 6.6mol), anhydrous dimethyl sulfoxide (780g, 10.0mol ), stirred and reacted at 60°C for 6 hours. (TCL tracking response). The reaction device was changed into a distillation device, vacuum distillation, the reduced pressure was 0.013 MPa, and 257 grams of colorless liquid with a boiling point of about 70° C. was collected. The content of the product measured by GC was 99.0%, and the yield was 95%. Under low temperature conditions, cyanuric fluoride is stored in containers made of polytetrafluoroethylene.

Embodiment 3

[0034] In a dry reaction vessel, add 1,3,5-trichloro-s-triazine (278g, 1.5mol) and tetrabutylammonium fluoride (1.57kg, 6.0mol), anhydrous dimethyl sulfoxide (702g, 9.0 mol), the reaction was stirred at 60°C for 6 hours. (TCL tracking response). The reaction device was changed into a distillation device, vacuum distillation, the reduced pressure was 0.013MPa, and 188 grams of colorless liquid with a boiling point of about 70° C. was collected. The content of the product measured by GC was 99.0%, and the yield was 93%. Under low temperature conditions, cyanuric fluoride is stored in containers made of polytetrafluoroethylene.

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 discloses a cyanuric fluoride preparation method. According to the method, 1, 3, 5-trichlorine s-triazine and tetrabutylammonium fluoride are subjected to fluorination to obtain cyanuricfluoride and tetrabutylammonium chloride. Catalysts are omitted, reaction selectivity is high, yield can reach up to 95%, usage of hydrogen fluoride serving as a high-risk fluorine reagent or a largequantity of metal fluoride and addition of expensive catalysts are avoided, and the method has the advantages of simplicity in operation, mild reaction conditions, low cost and the like, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a preparation method of cyanuric fluoride, in particular to a method for efficiently fluorinating 1,3,5-trichloro-s-triazine into cyanuric fluoride by using tetrabutylammonium fluoride as a fluorinating reagent, belonging to Fine chemical industry. Background technique [0002] Cyanuric fluoride, also known as 2,4,6-trifluoro-1,3,5-triazine, cyanuric fluoride, English name: Cyanuricfluoride, 2,4,6-trifluoro-1,3,5-triazine ( TFT). Molecular formula: C 3 f 3 N 3 , the structural formula: [0003] [0004] Trifluorocyanuric fluoride (TFT) is an important fluorinating reagent, which can react with carboxylic acid to generate acyl fluoride (J. Prakt. Chem. 2000, 342, 7, 711-714.). Cyanuric fluoride is an important intermediate of dyes and medicines, and it is a key intermediate for the synthesis of fluoro-s-triazine reactive dyes (EP Patent 1207186 and J Supercrit Fluids 40:477-484.). Because the fluorine atoms wit...

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): C07D251/28
CPCC07D251/28
Inventor 严楠余潇兵邱静茹廖维林郭晓红
Owner JIANGXI NORMAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com