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A kind of preparation method of formaldehyde-free sulfone bridge type syntan

A technology of sulfone bridge and formaldehyde, which is applied in the field of preparation of formaldehyde-free sulfone bridge syntans to achieve good light fastness

Active Publication Date: 2021-09-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no patents and literature reports on the use of cyanuric chloride instead of formaldehyde as a linker between the aromatic rings of sulfone bridge syntans to synthesize highly active sulfone bridge syntans

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Accurately weigh 0.1 mol of cyanuric chloride and place it in a 250 mL three-necked flask filled with acetone, keeping the internal temperature at 0 oC , dropwise add 0.2 mol 3,5-diaminobenzoic acid alkali solution, and at the same time dropwise add a mass concentration of 10% sodium hydroxide solution to control the reaction pH to 6.0, stir the reaction for 5.0 h; suction filter, and wash repeatedly with acetone Multiple times, vacuum drying for 5.0 h, after grinding to obtain intermediate A; increase the reaction temperature to 40 o C, add 0.2 mol of intermediate A to the three-necked flask, fully dissolve in distilled water, and under constant stirring, control the molar ratio of 4,4'-diaminodiphenylsulfone and intermediate A to 0.5: 1, slowly Add dropwise 4,4'-diaminodiphenylsulfone dissolved in acetone, and at the same time add dropwise 10% sodium hydroxide solution to control the reaction pH to 7.0, and continue the reaction for 8.0 h after the dropwise addition; ...

Embodiment 2

[0026] Accurately weigh 0.1 mol of cyanuric chloride and place it in a 250 mL three-necked flask filled with acetone, keeping the internal temperature at 0 oC , dropwise add 0.2 mol 4,4`-diaminostilbene-disulfonic acid alkali solution, and at the same time dropwise add 10% sodium carbonate solution to control the reaction pH to 6.0, stir for 5.0 h; , and repeatedly washed with acetone, dried in vacuum for 5.0h, and obtained intermediate A after grinding; raise the reaction temperature to 40 o C, add 0.2 mol of intermediate A to the three-necked flask, fully dissolve in distilled water, and under constant stirring, control the molar ratio of 4,4'-dihydroxydiphenyl sulfone and intermediate A to 0.65:1, slowly Add dropwise 4,4'-dihydroxydiphenyl sulfone dissolved in ether, and at the same time add dropwise 10% sodium carbonate solution to control the reaction pH to 7.0, and continue to react for 8.0 h after the dropwise addition; suction filtration, and repeat with ether After w...

Embodiment 3

[0028] Accurately weigh 0.1 mol of cyanuric chloride and place it in a 250 mL three-necked flask filled with acetone, keeping the internal temperature at 0 oC , dropwise add 0.2 mol aqueous solution of p-phenylenediamine sulfate, and at the same time dropwise add potassium carbonate solution with a mass concentration of 10% to control the reaction pH to 6.0, stir and react for 5.0 h; filter with suction, wash repeatedly with acetone, vacuum After drying for 5.0 h, intermediate A was obtained after grinding; the reaction temperature was increased to 40 o C, add 0.2 mol of intermediate A to the three-necked flask, fully dissolve in distilled water, and under constant stirring, control the molar ratio of 3,3'-diaminodiphenylsulfone and intermediate A to 0.75: 1, slowly Add dropwise 3,3'-diaminodiphenylsulfone dissolved in ether, and at the same time add dropwise potassium carbonate solution with a mass concentration of 10% to control the reaction pH to 7.0, and continue to react ...

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PUM

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Abstract

The invention discloses a preparation method of a formaldehyde-free sulfone bridge type syntan. First, keep the internal temperature at 0-5 oC , take cyanuric chloride as reaction substrate, and synthesize intermediate A through nucleophilic substitution reaction with bisamino-containing hydrophilic compound; then increase the temperature to 30~40 o C, controlling the molar ratio of the diphenyl sulfone compound to the intermediate A to be (0.5-1):1, and preparing a formaldehyde-free sulfone-bridged syntan with a molecular weight of 500-3000 through polycondensation reaction. The present invention adopts cyanuric chloride as linking agent between aromatic rings of sulfone bridge type syntans, completely eliminates pollution caused by free formaldehyde in sulfone bridge type syntans tanned leather, and introduces carbon-chlorine bond, imino group, sulfonate Active groups such as acid groups and more conjugated structures make it relatively more active, endowing crust leather with good moisture and heat resistance stability and light resistance.

Description

technical field [0001] The invention relates to a preparation method of a formaldehyde-free sulfone bridge type syntan, and specifically belongs to the technical field of synthesis of leather chemical tanning agents. Background technique [0002] As early as the end of the 18th century, Italian Schniff and others began to study syntans; in 1911, Professor E∙stiasny of Germany synthesized phenolsulfonic acid formaldehyde condensate and applied for a patent, and then transferred the technology to BASF company, which was first applied in practice In production; since then, research in this field has been carried out one after another around the world. After the Second World War, Bergman-Grassmos of Germany compiled the patents of various countries into a book, which made a systematic understanding of syntans; until now, nearly 100 The development history of many years shows that syntans have developed into the most varieties of special materials for leather and become an indisp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C14C3/08
CPCC14C3/08
Inventor 林炜肖远航梁玉可吴晓波
Owner SICHUAN UNIV