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Method for preparing triblock non-ionic fluorine-containing short-chain surfactant by non-isocyanate route

A non-isocyanate, surfactant technology, applied in the field of surfactant preparation, can solve the problem that the synthesis research of fluorine-containing short-chain surfactant has not been reported, and achieve excellent micelle stability and self-assembly performance, preparation Simple method, good biocompatibility and effect of biodegradability

Active Publication Date: 2020-05-12
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] However, after reviewing the data, it was found that the non-isocyanate route synthesis of fluorine-containing short-chain surfactants has not yet been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Place the activated 3A molecular sieve in heptafluorobutylamine, seal it overnight, and remove moisture; decompress polyethylene glycol diglycidyl ether at 100~120°C and a vacuum of 0.009MPa Distill to remove water; dry the three-necked bottle, agitator, and feeding tube at 100-120°C for 2-4 hours, take it out and place it in a desiccator to cool; add 30g of Polyethylene glycol diglycidyl ether, 0.92g tetrabutylammonium iodide, 0.59g perfluorinated tert-butanol, 12g carbon dioxide was introduced until the pressure reached 100 bar, and then the temperature was raised to 80°C for 16 hours to obtain a crude product; Treat the crude product under vacuum at 60°C for 16 hours to remove residual carbon dioxide and high-fluoro-tert-butanol to obtain a prepolymer; add 1.50 g of prepolymer and 1.00 g of Heptaflubutamine, heated to 50-70 ℃ with stirring, reacted for 6-8 hours; cooled to below 40 ℃, added a certain amount of distilled water and stirred for 0.5 hours, and...

Embodiment 2

[0040] Example 2: Place the activated 3A molecular sieve in heptafluorobutylamine, seal it overnight, and remove moisture; decompress polyethylene glycol diglycidyl ether at 100~120°C and a vacuum of 0.009MPa Distill to remove water; dry the three-necked bottle, stirrer, and feeding tube at 100-120°C for 2-4 hours, take it out and place it in a desiccator to cool; add 24g of 400 mol. Polyethylene glycol diglycidyl ether, 0.92g tetrabutylammonium iodide, 0.59g perfluorinated tert-butanol, 12g carbon dioxide was introduced until the pressure reached 100 bar, and then the temperature was raised to 80°C for 16 hours to obtain a crude product; Treat the crude product under vacuum at 60°C for 16 hours to remove residual carbon dioxide and high-fluoro-tert-butanol to obtain a prepolymer; add 1.50 g of prepolymer and 1.20 g of Heptaflubutamine, heated to 50-70 ℃ with stirring, reacted for 6-8 hours; cooled to below 40 ℃, added a certain amount of distilled water and stirred for 0.5 ho...

Embodiment 3

[0041] Example 3: Place the activated 3A molecular sieve in nonafluoropentylamine, seal it overnight, and remove moisture; decompress polyethylene glycol diglycidyl ether at 100~120°C and a vacuum of 0.009MPa Distill to remove water; dry the three-necked bottle, agitator, and feeding tube at 100-120°C for 2-4 hours, take it out and place it in a desiccator to cool; add 30g of Polyethylene glycol diglycidyl ether, 0.92g tetrabutylammonium iodide, 0.59g perfluorinated tert-butanol, 12g carbon dioxide was introduced until the pressure reached 100 bar, and then the temperature was raised to 80°C for 16 hours to obtain a crude product; Treat the crude product under vacuum at 60°C for 16 hours to remove residual carbon dioxide and high-fluorine tert-butanol to obtain a prepolymer; add 1.50 g of prepolymer and 1.25 g of Nonafluoropentylamine, heated to 50-70 °C under stirring, reacted for 6-8 hours; cooled to below 40 °C, added a certain amount of distilled water and stirred for 0.5 ...

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Abstract

The invention discloses a method for preparing a triblock non-ionic fluorine-containing short-chain surfactant through a non-isocyanate route. The triblock non-ionic fluorine-containing short-chain surfactant is prepared by the following steps: firstly, carrying out a reaction between polyethylene glycol diglycidyl ether and carbon dioxide at an equimolar ratio under the co-catalysis of tetrabutylammonium iodide and high-fluorine tert-butyl alcohol to obtain a prepolymer with cyclic carbonates at two ends, and then performing a ring-opening reaction between the prepolymer and short-chain fluoroamine to obtain the triblock non-ionic fluorine-containing short-chain surfactant. The preparation method is characterized in that a cyclic carbonate route is used for replacing an isocyanate route to synthesize a polyurethane structure, so that the non-isocyanate route synthesis of the triblock non-ionic fluorine-containing short-chain surfactant containing the polyurethane structure is realized, and the use of toxic isocyanate monomers is avoided. Besides, the preparation method of the triblock non-ionic fluorine-containing short-chain surfactant is simple, the surface activity is excellent, and the triblock non-ionic fluorine-containing short-chain surfactant has very good biocompatibility and biodegradability and has a wide application prospect.

Description

technical field [0001] The invention relates to a preparation method of a surfactant, in particular to a method for preparing a three-block nonionic fluorine-containing short-chain surfactant through a non-isocyanate route. Background technique [0002] Fluorosurfactant is a kind of special surfactant with fluorocarbon chain as hydrophobic chain. Chemically stable and both water and oil repellent. Due to these excellent properties, fluorine-containing surfactants are widely used in various fields such as fire protection, chemical industry, pesticides, mineral processing, papermaking, leather, textiles, and medicine. [0003] However, studies have shown that traditional long-chain fluorosurfactants represented by perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) have high toxicity and bioaccumulation and are difficult to degrade in the environment for a long time, resulting in a series of environmental problems. Therefore, in 2009, the United Nations En...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G71/04B01F17/00C09K23/00
CPCC08G71/04C09K23/16
Inventor 金勇周毓棠金泓宇
Owner SICHUAN UNIV
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